Share a compound : 7270-63-5

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Diazo-2,2-dimethyl-1,3-dioxane-4,6-dione, its application will become more common.

7270-63-5,Some common heterocyclic compound, 7270-63-5, name is 5-Diazo-2,2-dimethyl-1,3-dioxane-4,6-dione, molecular formula is C6H6N2O4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: To a solution of diazo compound 1 (0.5 mmol) and alkynes (1.1 mmol) in toluene (2 mL) was added rhodium(II) pivalate (0.01 mmol). The reaction mixture was stirred at 60C for 0.5-5 h. The solvent was evaporated in rotary evaporator under reduced pressure to give the residue. The residue was purified by flash column chromatography on silica gel to give the product. 4.2.17. 2,4-Di(phenanthren-9-yl)-6H-furo[2,3-b]pyran-6-one (5p). Reaction of 1 (85 mg, 0.5 mmol) and 9-ethynylphenanthrene (222 mg, 1.1 mmol) under Rh2(OPiv)4 (6 mg, 0.01 mmol) afforded 5p (98 mg, 40%) as a solid: mp 156-158 C; 1H NMR (300 MHz, CDCl3) delta 8.81-8.62 (4H, m), 8.23 (1H, d, J=7.5 Hz), 8.04-7.85 (5H, m), 7.78-7.53 (8H, m), 6.52 (1H, s), 6.42 (1H, s); 13C NMR (75 MHz, CDCl3) delta 159.3, 158.4, 154.2, 147.8, 131.8, 130.7, 130.6, 130.5, 130.5, 130.2, 129.1, 129.0, 128.8, 128.5, 128.4, 128.0, 127.9, 127.5, 127.4, 127.2, 127.1, 126.9, 126.9, 126.8, 126.7, 125.9, 125.3, 124.8, 123.1, 122.9, 122.5, 122.3, 107.5, 106.0, 101.3; IR (KBr) 2923, 1714, 1646, 1533, 1411, 1266, 1166, 1032, 962, 826, 750 cm-1; HRMS m/z (M+) calcd for C35H20O3: 488.1412. Found: 488.1411.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Diazo-2,2-dimethyl-1,3-dioxane-4,6-dione, its application will become more common.

Reference:
Article; Somai Magar, Krishna Bahadur; Lee, Yong Rok; Kim, Sung Hong; Tetrahedron; vol. 69; 44; (2013); p. 9294 – 9302;,
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Research on new synthetic routes about 42122-44-1

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 42122-44-1.

These common heterocyclic compound, 42122-44-1, name is Methyl 3-(4-fluorophenyl)propiolate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 42122-44-1

To a stirred solution of the product of Step AD2 (9 g, 0.05M) in dry toluene (90 ml) under nitrogen, nitro ethane (8.5 ml, 0.050M) was added, followed by triethylamine (3.4 ml, 0.025M). Then a solution of phenyl isocyanate (6 g, 0.05M) in dry toluene was added to the RM at 80 C. After the addition was over the stirring was continued for overnight at 80 C. The RM was cooled under ice bath, filtered and the filtrate was concentrated under vacuum. The resulting mass was taken in ethyl acetate (75 ml) and washed with water (2¡Á20 ml), 5% NH4OH (40 ml), dried over anhydrous sodium sulphate and concentrated under vacuum to get crude product which was purified by column chromatography over silica gel (60-120) using PE/EtOAC (9.9/0.1) as eluent to afford isoxazole ester 3.7 g (32%).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 42122-44-1.

Reference:
Patent; Gerritz, Samuel; Shi, Shuhao; Zhu, Shirong; US2006/287287; (2006); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

The important role of 111-82-0

The synthetic route of 111-82-0 has been constantly updated, and we look forward to future research findings.

111-82-0, A common heterocyclic compound, 111-82-0, name is Methyl laurate, molecular formula is C13H26O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

laurateMethyl laurate (99.4%, 870 mg, Wako Pure Chemical Industries,Ltd.), Ru-Sn-Mo/C catalyst (43 mg), Fe (28 mmol (1564 mg)of 60-80 nm particles without previous activation), H2O(28-83 mmol), and tetradecane were introduced into a 100 mLHastelloy C high pressure reactor. After purging the reactor fourtimes with nitrogen, it was heated to the required temperatureand maintained at that state for 1-24 h. The stirring rate wasadjusted to 1000 rpm. The resulting products were separated bycentrifugation and filtration, and their yields were determinedby gas chromatography on an instrument equipped with a flameionization detector (Shimadzu, GC-2014) using anisole as aninternal standard. A capillary column (Restek, Stabilwax) wasused to analyze the esters, alcohols, acids, and higher molecularweight hydrocarbons. The conversion of methyl laurate and yieldof product were defined as follows:

The synthetic route of 111-82-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sagata, Kunimasa; Hirose, Mina; Hirano, Yoshiaki; Kita, Yuichi; Applied Catalysis A: General; vol. 523; (2016); p. 85 – 91;,
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Analyzing the synthesis route of 64113-91-3

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 64113-91-3.

64113-91-3, These common heterocyclic compound, 64113-91-3, name is tert-Butyl 2-aminobenzoate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A 12 L round bottom flask, equipped with a thermocouple, nitrogen adapter and a 1 L addition funnel, was charged with a solution [OF T-BUTYL 2-AMINOBENZOATE] (537g, 2.78 moles; lot 36648-tjb-40) in ethanol (1620 [ML,] 3 ml/g). To this golden solution was added water (615.6 [ML)] resulting in a biphasic mixture. This mixture was cooled to between 15 and 20 C with a cold-water bath. A 1.0 M solution of [ICL IN CHZCIZ] [(ALDRICH LOT #14127JO,] 3.11 L, 3.11 moles, 1.12 equiv. ) was charged in portions to the addition funnel and was added to the rapidly stirred mixture maintaining the temperature between 15 and [25 C.] The addition time was 2.25 hours and the temperature range observed was 16.5 to 20. [4 C.] The resulting red brown mixture was stirred at room temperature for 1 hour at which time the GC assay showed the reaction was complete. The reaction was diluted with 920 mL of water and quenched with 456 mL of [38%] aq. sodium bisulfite (Webb [CHEM LOT #10464519)] resulting in a slight exotherm to 24. [0 C.] This mixture was stirred for 15 minutes before separating the phases. The methylene chloride layer was combined with water (3.7L) and stirred for 15 minutes before separating the phases. A [NAOH] solution was prepared by diluting 10% [NAOH] [(460ML)] in water (2.3L). To the methylene chloride layer was added this dilute [NAOH] solution (2.1L). The pH of the basic phase was 6.56. The phases were separated and the methylene chloride layer was concentrated to a low volume in vacuo at 16 torr using a bath temp of [45 C. PYRIDINE] (4L) was added, and the resulting solution was concentrated to ca. 1.0 mL/g [IN.] vacuo at 16 torr using a [62 C] water bath. The low volume pyridine/product mixture was diluted with pyridine to the target volume of 3. 1L (3. [5 ML/G).] A sample [(LOML)] was concentrated removing the pyridine on the rotovap and high vacuum to yield 3.12 g of an orange brown solid of 96% potecy by GC. GC assay of pyridine solution indicated that neither EtOH nor methylene chloride were present, so the solution was taken on directly into the next step.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 64113-91-3.

Reference:
Patent; PHARMACIA & UPJOHN COMPANY; WO2004/18414; (2004); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

The important role of 42726-73-8

Statistics shows that tert-Butyl methyl malonate is playing an increasingly important role. we look forward to future research findings about 42726-73-8.

42726-73-8, Name is tert-Butyl methyl malonate, 42726-73-8, belongs to esters-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows.

Potassium hydroxide (2.00 g, 36.0 mmol), tert-butyl methyl malonate (1.22 mL, 7.2 mmol) and DCM (20 mL) were added to a 100-mL flask under inert atmosphere. The mixture was stirred at room temperature until the solution became white then PhI(OAc)2 (1.93 g, 6.0 mmol) was added and stirred at room temperature for 2 hours. The solution was filtered through a cotton plug and washed with small portions of DCM. The solvent was removed under reduced pressure and the remaining oil was placed under high vacuum for 2 hours. The oil crystallized and the resulting solid was used without further purification. 1.038 g (46percent); off-white solid; m.p. 95-97¡ãC (dec.); 1H NMR (CDCl3; 600 MHz): delta 1.45 (s, 9H), 3.77 (s, 3H), 7.40-7.43 (m, 2H), 7.52-7.54 (m, 1H), 7.71-7.73 (m, 2H); 13C NMR (CDCl3; 150 MHz): delta 28.6, 52.5, 80.1, 114.5, 127.5, 130.3, 131.3, 131.5, 163.9, 164.4; HRMS: Calculated for C14H18IO4 (377.0250) [M+H]+, Found: 377.0255.

Statistics shows that tert-Butyl methyl malonate is playing an increasingly important role. we look forward to future research findings about 42726-73-8.

Reference:
Article; Stokes, Sean; Mustain, Rachel; Pickle, Lydia; Mead, Keith T.; Tetrahedron Letters; vol. 53; 30; (2012); p. 3890 – 3893;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics