反应详情

A solution of 8.73 g (32.4 mmol) of tert.-butyl 3-(thiazol-2-ylamino)pyrrolidine-1-carboxylate (synthesis described in Example 11) in MeCN (120 ml) was combined with 1.56 g (38.9 mmol, 60% strength in mineral oil) of sodium hydride and stirred for 30 min at RT. 4.04 ml (64.8 mmol) of iodomethane were then added and stirring was continued for a further 3 h at RT. After addition of a conc. aq. NH4OH soln. (30 ml), the phases were separated and the aqueous phase was extracted with EA. The collected organic phases were dried over MgSO4, filtered and evaporated under a vacuum. 3.16 g (11.2 mmol, 34%) of tert.-butyl 3-(methyl(thiazol-2-yl)amino)pyrrolidine-1-carboxylate were obtained by CC (chloroform/EA 20:1) with the residue.

1. stirringstirring
2. waitwas continued for a further 3 h at RT
3. custom(30 ml), the phases were separated
4. extractionthe aqueous phase was extracted with EA
5. dry with materialThe collected organic phases were dried over MgSO4
6. filtrationfiltered
7. customevaporated under a vacuum