반응 #90850

ord-3c91b85feed141eba2da4cf9e8233326

반응 방정식

N[C@H](CO)C(=O)O
D-serine
CC(=O)Cl
Acetyl chloride
COC(=O)[C@H](N)CO.Cl
D-serine methyl ester hydrochloride
수율 91.0%

시약

없음

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

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%)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447024B1uspto-grants-2016_09