反应详情

A solution of 80 mg (0.23 mmol) of trans-(1E)-[4-(3-Chloro-propenyl)-cyclohexyl]-methyl-carbamic acid 4-chloro-phenyl ester in 4.3 ml of methanol was treated with 0.24 ml (2.34 mmol) N-methylpropylamine and stirred over night at RT. The solvent was evaporated and the residue extracted with aqueous saturated NaHCO3/Et2O (3×). The organic phase was dried with Na2SO4, filtered and evaporated. Purification by flash column chromatography on silica gel (CH2Cl2/MeOH 95:5) gave 46 mg (52%) of trans-(1E)-Methyl-{4-[3-(methyl-propyl-amino)-propenyl]-cyclohexyl}-carbamic acid 4-chloro-phenyl ester, MS: 379 (MH+, 1Cl).

1. customThe solvent was evaporated
2. extractionthe residue extracted with aqueous saturated NaHCO3/Et2O (3×)
3. dry with materialThe organic phase was dried with Na2SO4
4. filtrationfiltered
5. customevaporated
6. customPurification by flash column chromatography on silica gel (CH2Cl2/MeOH 95:5)