Tag: M.W=100-200

A common heterocyclic compound, 680-65-9, name is Diethyl difluoromalonate, molecular formula is C7H10F2O4, 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. 680-65-9.

Step 1: Procedure for preparation of Compound 9bTo a solution of NH3/MeOH (sat., 50 mL) was added compound 9a (5 g, 25.5 mmol) at -78 C and stirred at this temperature for 2 h. Then the reaction mixture was allowed to warm to room temperature slowly and stirred overnight. The reaction mixture was concentrated under reduced pressure to dryness to give compound 9b (3.3 g, 94%) as a white solid.1H NMR (DMSO-dtf 400 MHz): delta 8.24 (br, 2H), 8.09 (br, 2H).

The synthetic route of Diethyl difluoromalonate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DILLARD, Lawrence W.; YUAN, Jing; LEFTHERIS, Katerina; VENKATRAMAN, Shankar; WU, Guosheng; JIA, Lanqi; XU, Zhenrong; CACATIAN, Salvacion; MORALES-RAMOS, Angel; SINGH, Suresh; ZHENG, Yajun; WO2011/106414; (2011); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 344-14-9, name is Dimethyl 2-fluoromalonate, belongs to esters-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 344-14-9, 344-14-9

A. Preparation of 5-Fluoro-4,6-dihydroxy-2-pyrimidineamine (3) Sodium (257 mg, 11 mmol) was dissolved in absolute ethanol (50 ml) with stirring under argon. When the sodium had thoroughly dissolved, guanidine hydrochloride (2) (502 mg, 5 mmol) and diethyl fluoromalonate (1) (790 mg, 4.4 mmol) were added. The solution was left to stir at room temperature overnight. A condenser was then attached to the flask and the solution was refluxed under argon for 4.5 hours. The solution was cooled to room temperature and concentrated. The residue was redissolved in 20 ml hot H2 O and acidified to pH 4. The mixture was cooled on ice and the precipitate was collected, yielding (3) as a peach colored solid (618 mg, 96%): MS (70 eV, EI)m/z (relative intensity) 146(M+, 100), 18 (95), 172 (26), 17 (24), 300 (21); IR (mull, cm-1) 3363, 1695, 1601, 1420, 1208, 677, 666; UV (MeOH, nm) 206(3,840), 235(3,380), 270(11,600). Exact Mass Calcd for C4 H4 N3 O2 F: 146.0366. Found: 146.0371.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Dimethyl 2-fluoromalonate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; The Upjohn Company; US5373012; (1994); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 584-74-7 name is Ethyl 2-fluorophenylacetate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 584-74-7

At -78 C., DIBAL-H (1 M in toluene, 125 ml, 0.125 mol) was added dropwise to a solution of ethyl 2-fluorophenylacetate (22.7 g) in toluene (90 ml). After the addition, the mixture was stirred at this temperature for another 3 hours, and MeOH (90 ml) was then added dropwise. The suspension was poured into hydrochloric acid (2 M, 400 ml) and extracted with MTBE (3¡Á300 ml). The combined organic phases were dried over sodium sulfate and concentrated. This gave 16.2 g of the desired product as a colorless oil (94%). 1H NMR (300 MHz, CDCl3) delta 9.76 (s, 1H), 7.34-7.07 (m, 4H), 3.73 (m, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 2-fluorophenylacetate, and friends who are interested can also refer to it.

Reference:
Patent; BASF SE; US2011/172097; (2011); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics