Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 35179-98-7, name is Chloromethyl ethyl carbonate, A new synthetic method of this compound is introduced below., SDS of cas: 35179-98-7
Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 35179-98-7, name is Chloromethyl ethyl carbonate, A new synthetic method of this compound is introduced below., SDS of cas: 35179-98-7
Sodium IODIDE (25 MG) was dissolved in acetonitrile (0. 15 mL) in which had been dissolved chloromethyl ethyl carbonate (22 mg) [Z. Li et al. , Bioorg. Med. CHEM. LETT., 7,2909 (1997)], and the solution was stirred for four hours under dark room conditions at room temperature. Next, the solution was added to DMF (0. 30 mL) in which had been dissolved BOC–ALA-HIS (TRT) (30 mg) and DIISOPROPYLETHYLAMINE (0. 019 ML), and stirring was further carried out for 3 days at room temperature. After that, ethyl acetate (30 mL) was added to the solution obtained, and the solution was washed with a sodium hydrogencarbonate aqueous solution (5 mL) twice and a sodium chloride aqueous solution (5 ML) once. After the washing, drying was carried out with sodium sulfate, concentration was carried out under reduced pressure, the concentrate was dissolved in a mixed liquid of acetonitrile and water (1: 4), and then freeze drying was carried out, thus obtaining A white powder (approximately 55 mg). The powder was treated for 30 minutes with TFA (1.2 ML) CONTAINING 2% TRIISOPROYLSILANE and 2% water, and then washing was carried out three times with ether (10 mL). The residue was dissolved in a mixed solution of acetonitrile and water (1: 4), and then freeze drying was carried out, thus obtaining 28 mg of crude product. The crude product obtained was subjected to HPLC (with an ODS column) with the undermentioned conditions using water- acetonitrile containing 0. 1T TFA as an eluent, the fraction containing THE TARQET COMPOUND (ss-ALA-HIS-OCH2-OCO-OCH2CH3) was isolated using the absorbance at 220 nm as an indicator, and freeze drying was carried out, thus obtaining a white powder (19 mg) of P-ALA-HIS-OCH2-OCO-OCH2CH3 (TFA salt). This powder was dissolved in a 0. 05 M HC1 aqueous solution containing 5% acetonitrile, and freeze drying was again carried out, whereby the target compound (-ALA-HIS-OCH2-OCO-OCH2CH3 2HC1) WAS obtained as a white powder (11 mg, 52T yield). LT;HPLC CONDITIONS GT; Column : Cosmosil 5C18-MS 10 x 250 mm Eluent : Solution A: Water containing 0. 1% TFA Solution B: Acetonitrile containing 0. 1% TFA Concentration gradient Time (min) 0 20 25 Solution B % 5 15 95 Flow rate : 2.5 ML/MIN -H NMR (400 MHz, DMSO-d6, 25C) : No. 1. 23 (3H, t, J = 7.1 Hz), 2.46-2. 58 (2H, m), 2. 88-2. 98 (2H, m), 3.07 (1H, dd, J = 8.8 and 15.1 Hz), 3.16 (1H, dd, J = 5.7 and 15. 1 Hz), 4.19 (2H, q, J = 7.1 Hz), 4.58-4. 66 (1H, m), 5.69 (1H, d, J = 6.1 Hz), 5.72 (1H, d, J = 6. 1 HZ), 7.44 (1H, s), 7. 87 (3H, br), 8.87 (1H, d, J = 7.2 Hz), 9. 01 (1H, S), 14.35 (2H, br) ; DUC NOR (100 MHz, DMSO-DS, 25C) : 8 13.9, 25. 6,31. 8,34. 9, 51.3, 64.5, 82.4, 117. 2, 128.6, 133.9, 153.1, 169. 3, 169. 8; ESI-MS: m/z 329 (M+H) ; calculated for CL3H2LN406 : 329.
The synthetic route of 35179-98-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; OSAKA INDUSTRIAL PROMOTION ORGANIZATION; OSAKA UNIVERSITY; WO2005/9471; (2005); A1;,
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