反应详情

温度

100 °C

To 1.72 g (4.58 mmol) trans-Methanesulfonic acid 4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexylmethyl ester in 17 ml DMF, 0.78 g (6.86 mmol, 1.5 eq) potassium thioacetate were added and the mixture was heated to 100° C. for 10 min. The mixture was concentrated under vacuum and the residue was dissolved in saturated NaHCO3/Et2O (3×). The organic phases were washed with brine, dried over Na2SO4 and evaporated to yield 1.69 g (quantitative) of trans-Thioacetic acid S-{4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexylmethyl}ester, MS: 356 (MH+).

1. concentrationThe mixture was concentrated under vacuum
2. dissolutionthe residue was dissolved in saturated NaHCO3/Et2O (3×)
3. washThe organic phases were washed with brine
4. dry with materialdried over Na2SO4
5. customevaporated