反应详情

A mixture of 4-tert-butoxycarbonylamino-cyclohexanecarboxylic acid (2.43 g, 10 mmol), EDCI (6.52 g, 34 mmol) and HOBt (4.59 g, 34 mmol) in NMP (20 mL) was stirred at RT for 3 h. A solution of dimethylamine (2.0 M in THF, 15 mL, 30 mmol) was added, and the resulting mixture was stirred at RT for 64 h. Water and EtOAc were then added, and the organic layer was separated and washed twice with a saturated aqueous solution of K2CO3, aqueous HCl (1 M), a saturated aqueous solution of K2CO3, and brine. The organic layer was dried over Na2SO4, filtered and evaporated under reduced pressure to give (4-dimethylcarbamoyl-cyclohexyl)-carbamic acid tert-butyl ester (1.6 g, 59% yield) as a white solid.

1. stirringthe resulting mixture was stirred at RT for 64 h
2. customthe organic layer was separated
3. washwashed twice with a saturated aqueous solution of K2CO3, aqueous HCl (1 M)
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. customevaporated under reduced pressure