反应详情

To a solution of 2-chloro-5-nitrobenzaldehyde (25 g) in EtOH (200 mL) was added 3-methylallylamine (10.6 g, 1.1 eq). HOAc (9 g) was added to the solution. The mixture was stirred at 20˜25° C. for 3 h. NaBH(OAc)3 (43 g, 1.5 eq) was added in one portion at ˜5° C. The mixture was warmed to RT in 30 min and stirred for 1 h. The EtOH was removed under reduced pressure and saturated Na2CO3 aqueous solution (200 mL) was added. The mixture was extracted with toluene (100 mL). To the toluene solution was added 5 N HCl in IPA (20 mL) at ˜5° C. in 1 h. The mixture was stirred for 1 h. The solids were filtered off, and dried under vacuum.

1. stirringstirred for 1 h
2. customThe EtOH was removed under reduced pressure and saturated Na2CO3 aqueous solution (200 mL)
3. additionwas added
4. extractionThe mixture was extracted with toluene (100 mL)
5. additionTo the toluene solution was added 5 N HCl in IPA (20 mL) at ˜5° C. in 1 h
6. stirringThe mixture was stirred for 1 h
7. filtrationThe solids were filtered off
8. customdried under vacuum