HRID26997

反应详情

EQUATION

反应方程式

HRID 26997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of o-aminomethylphenylacetic acid hydrochloride (7.50 g., 37 m.mol.) and sodium hydroxide (4.74 g., 118 m.mol.) in water (100 ml.) was added p-toluenesulfonyl chloride (7.64 g., 40 m.mol.) in portions at 60° C. The mixture was stirred for 1 hour at the same temperature and acidified with hydrochloric acid. The mixture was extracted with ethyl acetate (4×50 ml.). The combined extracts were washed with water, treated with a small amount of carbon and dried. The solvent was evaporated under reduced pressure and the residue crystallized from ethyl acetate to afford 2 as colorless prisms. Yield, 9.84 g. (84%). M.p. 155°-156° C.

WORKUP

后处理

  1. extractionThe mixture was extracted with ethyl acetate (4×50 ml.)
  2. washThe combined extracts were washed with water
  3. additiontreated with a small amount of carbon
  4. customdried
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue crystallized from ethyl acetate