HRID553422

反应详情

EQUATION

反应方程式

HRID 553422 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

31.1 g (130 mmol) of 5-acetyl-4,5,6,7-tetrahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester (C) were dissolved in 30 mL of EtOH and combined at RT with 30 mL (260 mmol) of 32% (weight percent) hydrochloric acid solution in water. After two hours' heating with refluxing, the solution was evaporated and introduced into 500 mL of cooled EtOAc (ice bath). The resultant precipitate was separated and dried under a vacuum. 8.13 g (27% of theoretical) of the desired product 4,5,6,7-tetrahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester hydrochloride (D) were obtained.

WORKUP

后处理

  1. temperatureAfter two hours' heating
  2. temperaturewith refluxing
  3. customthe solution was evaporated
  4. additionintroduced into 500 mL of cooled EtOAc (ice bath)
  5. customThe resultant precipitate was separated
  6. customdried under a vacuum