反应详情

Combine 6-mercapto-nicotinic acid (0.64 g, 4.1 mmol), benzylamine (0.45 mL, 4.1 mmol) and EEDQ (1 g, 4 mmol) in anhydrous DMF (3 mL). Stir at room temperature for 12 h. Dilute the reaction with water and extract with DCM. Dry over MgSO4, filter and concentrate in vacuo to give a yellow solid. Purify by chromatography on silica gel eluting with 2M ammonia in methanol/DCM (2:98 and 10:90) to give the title compound as a yellow solid (440 mg, 44%). MS (ES+) m/z: 245 (M+H)+.

1. additionDilute
2. extractionextract with DCM
3. dry with materialDry over MgSO4
4. filtrationfilter
5. concentrationconcentrate in vacuo
6. customto give a yellow solid
7. customPurify by chromatography on silica gel eluting with 2M ammonia in methanol/DCM (2:98 and 10:90)