반응 #578810

반응 방정식

NaBH(OAc)3

HOAc

2-chloro-5-nitrobenzaldehyde

3-methylallylamine

→

(2-Chloro-5-nitro-benzyl)-(2-methyl-allyl)-amine

용매

EtOH

반응 조건

후처리

1. 1
   workup.STIRRINGstirred for 1 h
2. 2
   기타The EtOH was removed under reduced pressure and saturated Na2CO3 aqueous solution (200 mL)
3. 3
   workup.ADDITIONwas added
4. 4
   추출The mixture was extracted with toluene (100 mL)
5. 5
   workup.ADDITIONTo the toluene solution was added 5 N HCl in IPA (20 mL) at ˜5° C. in 1 h
6. 6
   workup.STIRRINGThe mixture was stirred for 1 h
7. 7
   여과The solids were filtered off
8. 8
   기타dried under vacuum

실험 절차

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.

출처