HRID2375354

反应详情

EQUATION

反应方程式

HRID 2375354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(Trifluoroacetyl)-1,2,3,4-tetrahydroisoquinoline (140 mmol, 32.00 g) was introduced into CS2 (190 ml). Aluminum trichloride (837 mmol, 111.60 g) was added thereto in portions at room temperature. Acetyl chloride (419.12 mmol, 32.90 g) was then added dropwise in such a way that gentle refluxing took place, and the mixture was heated to reflux for a further hour. The reaction mixture was poured into ice-water and extracted with dichloromethane. The organic phase was dried, filtered with suction and concentrated and then stirred with isopropanol. 22 g of the title compound were obtained with a melting point of 80° C.

WORKUP

后处理

  1. customat room temperature
  2. temperaturethat gentle refluxing
  3. temperaturethe mixture was heated
  4. temperatureto reflux for a further hour
  5. extractionextracted with dichloromethane
  6. customThe organic phase was dried
  7. filtrationfiltered with suction
  8. concentrationconcentrated