반응 #630079

반응 방정식

2-amino-4-(3-nitrophenyl)butane

2,2-dimethyl-4-formyl-chroman

sodium boranate

→

4-{N-[4-(3-nitrophenyl)-2-butyl]-aminomethyl}-2,2-dimethylchroman

용매

methanol

반응 조건

후처리

1. 1
   workup.STIRRINGslight cooling, and the mixture is stirred for 1.5 hours
2. 2
   workup.STIRRINGstirring
3. 3
   기타the mixture is evaporated down
4. 4
   세척The ethyl acetate phase is washed with water
5. 5
   기타dried
6. 6
   기타evaporated down
7. 7
   workup.DISTILLATIONDistillation

실험 절차

12.1 g (0.1 mol) of 2-amino-4-(3-nitrophenyl)butane are added to 19.0 g (0.1 mol) of 2,2-dimethyl-4-formyl-chroman in 100 ml of methanol at 20° C., with stirring and slight cooling, and the mixture is stirred for 1.5 hours. Thereafter, 4.5 g of sodium boranate are added, and stirring is continued for 1 day, and the mixture is evaporated down and worked up with ethyl acetate/water. The ethyl acetate phase is washed with water, dried and evaporated down. Distillation gives 4-{N-[4-(3-nitrophenyl)-2-butyl]-aminomethyl}-2,2-dimethylchroman. B.p.: 225°-235° C./0.04 mmHg.

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