反应详情

607 mg (4.4 mmol) of K2CO3 were added to a solution of 500 mg (2.0 mmol) of 2-mercapto-N-(thiophen-2-ylmethyl)nicotinamide (V1) in DMF (5 ml), and the mixture was stirred for 1 h at RT. 446 mg of (2-bromoethyl)-(cyclohexyl)sulfane (crude product V2) were then added, and stirring was continued for a further 18 h at RT. The mixture was then diluted with ethyl acetate, and water was added. The phases were separated and the aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over MgSO4, filtered and concentrated in vacuo. CC (ethyl acetate/n-hexane 1:1) with the residue yielded 268 mg (0.68 mmol, 34%) of 2-(2-(cyclohexylthio)ethylthio)-N-(thiophen-2-ylmethyl)nicotinamide. MS: m/z 393.1 [M+H]+.

1. stirringstirring
2. waitwas continued for a further 18 h at RT
3. additionwas added
4. customThe phases were separated
5. extractionthe aqueous phase was extracted with ethyl acetate
6. dry with materialThe combined organic phases were dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo