反应详情

温度

85 °C

To a stirred solution of 2-methylene-3-quinuclidinone hydrochloride (0.5 g, 3.6 mmol) in water (6 ml) triethylamine (1.5 ml), tetra-n-butyl ammonium bromide (120 mg) and 6-mercapto-purine monohydrate (0.62 g) were added and the reaction mixture was allowed to stir at 85° C. for 14 h. The completion of reaction was monitored by tlc. The reaction mixture was quenched with ice-cold water (10 ml), extracted with dichloromethane (2×25 ml), the organic layers were washed with water, brine and dried over sodium sulphate, filtered and concentrated to get the crude product which was purified (140 mg, 14%) by flash column chromatography on neutral silica gel using 9:1 chloroform:methanol as eluent.

1. customThe completion of reaction
2. customThe reaction mixture was quenched with ice-cold water (10 ml)
3. extractionextracted with dichloromethane (2×25 ml)
4. washthe organic layers were washed with water, brine
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated