반응 #71532

반응 방정식

NaOH

cyclohexanecarbaldehyde

2,2-diethoxyethylamine

Sodium triacetoxyborohydride

→

N-cyclohexylmethyl-(2,2-diethoxyethyl)amine

용매

MeTHF

반응 조건

후처리

1. 1
   온도cooled to 0° C
2. 2
   workup.STIRRINGthe reaction mixture was stirred for 2 h
3. 3
   온도cooled to 0° C
4. 4
   세척The organic layer was washed with brine in water (1:1, 2×1 L)
5. 5
   workup.ADDITIONMeTHF (1 L) was added

실험 절차

To a mixture of 2,2-diethoxyethylamine (209 mL, 1.43 mol) and MeTHF (1050 L) was added cyclohexanecarbaldehyde (107 mL, 0.89 mol). The reaction mixture was stirred for 30 min at room temperature and cooled to 0° C. Sodium triacetoxyborohydride (378 g, 1.79 mol) was added over 40 min and the reaction mixture was stirred for 2 h and cooled to 0° C. 1 M NaOH (1 L) was added. The organic layer was washed with brine in water (1:1, 2×1 L) and the volume was reduced to ˜20%. MeTHF (1 L) was added and the volume reduced to ˜20%. The solution of the crude title intermediate was used directly in the next step.

출처