HRID2410657
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationwas concentrated
- dissolutionthe residue was dissolved in water
- additionAqueous 1M HCl was added to this solution until pH=5 whereupon a light yellow solid
- customprecipitated
- filtrationThe solid was collected by filtration
- washwashed with water
- customair-dried
- customsuch in the next reaction