반응 #53850

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trans-Methanesulfonic acid 4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexylmethyl ester

potassium thioacetate

→

trans-Thioacetic acid S-{4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexylmethyl} ester

수율 103.7%

용매

DMF

반응 조건

후처리

1. 1
   농축The mixture was concentrated under vacuum
2. 2
   workup.DISSOLUTIONthe residue was dissolved in saturated NaHCO3/Et2O(3×)
3. 3
   세척The organic phases were washed with brine
4. 4
   건조dried over Na2SO4
5. 5
   기타evaporated

실험 절차

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+).

출처