Acetyl chloride → D-Serine methyl ester hydrochloride

HRID 62572

반응식

HRID 62572 반응식
[NH2:1][C@@H:2]([C:5]([OH:7])=[O:6])[CH2:3][OH:4].[C:8]([Cl:11])(=O)C>CO>[ClH:11].[CH3:8][O:6][C:5](=[O:7])[C@@H:2]([CH2:3][OH:4])[NH2:1]

참가 물질

4

반응물 2

HCID 6367Acetyl chlorideHCID 71077D-Serine

생성물 1

HCID 11446470D-Serine methyl ester hydrochloride수율 91%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

D-serine (100 g, 0.9515 mole) was suspended in 600 ml methanol at room temperature. Acetyl chloride (224.0 g, 2.8545 mole) was added drop wise at −5° C. to 0° C. and stirred for 30 minutes. The reaction mixture was refluxed for 15 hours. Evaporation of the reaction mixture under reduced pressure followed by crystallization of the resulting residue from methanol and methyl tert-butyl ether, resulted in colorless solid of D-serine methyl ester hydrochloride (134.7 g, Yield: 91%, HPLC: 99.6%)

후처리

  1. temperatureThe reaction mixture was refluxed for 15 hours
  2. customEvaporation of the reaction mixture under reduced pressure
  3. customfollowed by crystallization of the resulting residue from methanol and methyl tert-butyl ether

출처 및 근거

ORD 기록
ord-3c91b85feed141eba2da4cf9e8233326
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447024B1

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