HRID1836102
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
2-(2,3,3a,8b-Tetrahydrocyclopenta[b]indol-4(1H)-yl)acetamide (90 mmol, 20 g) was dissolved in 1 M BH3.THF (200 mL) and heated to reflux for 18 h. The reaction mixture was allowed to cool to room temperature and then quenched slowly with methanol. The solution was concentrated, dissolved in methanol, and again concentrated. The resulting oil was diluted with ether and extracted twice with 1 N HCl. The aqueous phase was treated with 2.5 N NaOH to pH>10 and extracted with chloroform. The combined chloroform extracts were dried over MgSO4, filtered and concentrated to provide a yellow oil which was used without further purification.
WORKUP
后处理
- temperatureheated
- temperatureto reflux for 18 h
- customquenched slowly with methanol
- concentrationThe solution was concentrated
- dissolutiondissolved in methanol
- concentrationagain concentrated
- additionThe resulting oil was diluted with ether
- extractionextracted twice with 1 N HCl
- additionThe aqueous phase was treated with 2.5 N NaOH to pH>10
- extractionextracted with chloroform
- dry with materialThe combined chloroform extracts were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customto provide a yellow oil which
- customwas used without further purification