HRID51310
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 430 mg. of the product from Example 3 Part D, 2.0 gm. of 5% Pd/C, and 20 mL of carbitol was heated to reflux and refluxed for 21 hours, cooled, and filtered. The filtrate was diluted with water, acidified with hydrochloric acid, and extracted well with ethyl acetate. The organic phase was washed with brine, dried over sodium sulfate and evaporated in vacuo. The residue was triturated with dichloromethane and filtered to remove solid tetrahydrocarbazole. The filtrate was evaporated in vacuo to give the title product, 125 mg, 31%.
WORKUP
后处理
- additionA mixture of 430 mg
- temperatureto reflux
- temperaturerefluxed for 21 hours
- temperaturecooled
- filtrationfiltered
- additionThe filtrate was diluted with water
- extractionextracted well with ethyl acetate
- washThe organic phase was washed with brine
- dry with materialdried over sodium sulfate
- customevaporated in vacuo
- customThe residue was triturated with dichloromethane
- filtrationfiltered
- customto remove solid tetrahydrocarbazole
- customThe filtrate was evaporated in vacuo