反应详情

A solution of Trans-5-chloro-N-(4-hydroxymethyl-cyclohexyl)-2-methyl-nicotinamide (step 1) (100 mg, 0.354 mmol) and pyridine (3.6 ml) in dry DCM (3.5 ml) under nitrogen is cooled to approx. 0° C. using an ice-water bath. Methanesulfonyl chloride (0.030 ml, 0.389 mmol) is added dropwise. The reaction mixture is allowed to warm to room temp and stirred at this temp for 4 hours. The reaction is quenched by the addition of sat. NH4Cl at room temp and then extracted with diethyl ether (3×20 ml). The Et2O extracts are combined, washed with sat brine (20 mL), dried (MgSO4), filtered and evaporated to give the title compound as a colourless solid.

1. customThe reaction is quenched by the addition of sat. NH4Cl at room temp
2. extractionextracted with diethyl ether (3×20 ml)
3. washwashed with sat brine (20 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated