HRID2410657

反应详情

EQUATION

反应方程式

HRID 2410657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of ethyl 6-bromo-8-carbamoyl-2,3,4,9-tetrahydro-1H-carbazole-3-carboxylate (0.9 g, 2.464 mmol) and LiOH (0.177 g, 7.39 mmol) in THF/EtOH/H2O (3/1/1) (25 mL) was stirred at room temperature for 72 hours The reaction mixture was concentrated and the residue was dissolved in water. Aqueous 1M HCl was added to this solution until pH=5 whereupon a light yellow solid precipitated. The solid was collected by filtration, washed with water, air-dried and used as such in the next reaction. LCMS: RT=0.96 min, m/z (M+H) 337.0/339.0.

WORKUP

后处理

  1. concentrationwas concentrated
  2. dissolutionthe residue was dissolved in water
  3. additionAqueous 1M HCl was added to this solution until pH=5 whereupon a light yellow solid
  4. customprecipitated
  5. filtrationThe solid was collected by filtration
  6. washwashed with water
  7. customair-dried
  8. customsuch in the next reaction