HRID330594
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
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
In 8.5 ml of acetic acid introduced therein hydrogen chloride gas (400 mg, 11.0 mmol), 7a-cyano-2,3,5,6,7,7a-hexahydro-1H-pyrrolizine (300 mg, 2.20 mmol, obtained in Example 1) and platinum oxide (30 mg) were added to stir under hydrogen gas atmosphere for 24 hours at 20° C. After removal of insoluble matters from the reaction mixture, the filtrate was concentrated, 0.5N NaOH (10 ml) was added to the residue, which was extracted with chloroform, the extract was dried over anhydrous sodium sulfate, concentrated, and distilled in vacuo to afford 188 mg of the desired compound (Yield: 61%).
WORKUP
后处理
- customAfter removal of insoluble matters from the reaction mixture
- concentrationthe filtrate was concentrated
- addition0.5N NaOH (10 ml) was added to the residue, which
- extractionwas extracted with chloroform
- dry with materialthe extract was dried over anhydrous sodium sulfate
- concentrationconcentrated
- distillationdistilled in vacuo