反应详情

To the mixture obtained from Example 1, tosyl chloride (42 g) was added in portions with cooling. The resultant mixture was stirred for 5.5 hours, and then stood overnight. The solution was then poured into 4M hydrochloric acid (300 ml), stirred for 30 minutes, and then extracted with dichloromethane (×4). The combined extracts were washed with saturated brine, dried (magnesium sulphate) and evaporated to obtain the title compound as a dark red oil (30.95 g) 'H n.m.r. δ (CDCl3) 3.35(2H, d, J=7Hz, CH2CH), 3.55(2H,s,CH2CN), 4.77 (1H,t, J=7Hz, CH2CH).

1. temperaturewith cooling
2. extractionextracted with dichloromethane (×4)
3. washThe combined extracts were washed with saturated brine
4. dry with materialdried (magnesium sulphate)
5. customevaporated