HRID1464699

反应详情

EQUATION

反应方程式

HRID 1464699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

8-Bromo-3-nitrochroman (400 mg; 1.55 mmol) was dissolved in glacial acetic acid (30 ml) and zinc dust (2 g) was added. The mixture was heated to 100° C. for 15 minutes. The zinc dust was filtered off and washed with dichloromethane. The solvent was evaporated and the remaining oil extracted with diluted hydrochloric acid/dichloromethane. The phases were separated and the pH of the water layer was adjusted to 11 with 2N NaOH. The water layer was extracted with dichloro-methane. The phases were separated and the organic layer dried (Na2SO4). The solvent was evaporated yielding 214 mg (61%) of 8-bromo-3-aminochroman.

WORKUP

后处理

  1. filtrationThe zinc dust was filtered off
  2. washwashed with dichloromethane
  3. customThe solvent was evaporated
  4. extractionthe remaining oil extracted with diluted hydrochloric acid/dichloromethane
  5. customThe phases were separated
  6. extractionThe water layer was extracted with dichloro-methane
  7. customThe phases were separated
  8. dry with materialthe organic layer dried (Na2SO4)
  9. customThe solvent was evaporated