HRID916903

反应详情

EQUATION

反应方程式

HRID 916903 的结构方程式

PROCEDURE

实验过程

D-4-Hydroxyphenylglycine 11 (10.1 g, 60.4 mmol) was suspended in methanol (100 ml), and thionyl chloride (5.2 ml, 72.5 mmol) was added dropwise thereto at 50° C. over 0.5 hrs. After further keeping at 50° C. for 3 hrs, the solvent was distilled off under reduced pressure, and toluene and ethyl acetate were added to the residue. A resulting solid was collected by filtration and dried in vacuo to give D-4-hydroxyphenylglycine methyl ester hydrochloride 12 (12.5 g, yield 95.3%).

WORKUP

后处理

  1. waitAfter further keeping at 50° C. for 3 hrs
  2. distillationthe solvent was distilled off under reduced pressure, and toluene and ethyl acetate
  3. additionwere added to the residue
  4. filtrationA resulting solid was collected by filtration
  5. customdried in vacuo