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

HRID 542897

반응식

HRID 542897 반응식
[NH2:1][CH:2]([CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=1)[CH3:3].[CH3:15][C:16]1([CH3:28])[CH2:25][CH:24]([CH:26]=O)[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[O:17]1.B([O-])=O.[Na+]>CO>[N+:12]([C:8]1[CH:7]=[C:6]([CH2:5][CH2:4][CH:2]([NH:1][CH2:26][CH:24]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[O:17][C:16]([CH3:15])([CH3:28])[CH2:25]2)[CH3:3])[CH:11]=[CH:10][CH:9]=1)([O-:14])=[O:13]

참가 물질

5

반응물 3

HCID 145326Sodium metaborateHCID 135370432,2-Dimethyl-3,4-dihydro-2H-1-benzopyran-4-carbaldehydeHCID 135370444-(3-Nitrophenyl)butan-2-amine

생성물 1

HCID 135370454-{N-[4-(3-nitrophenyl)-2-butyl]-aminomethyl}-2,2-dimethylchroman

시약·촉매·용매 1

HCID 887Methanol용매

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.

후처리

  1. stirringslight cooling, and the mixture is stirred for 1.5 hours
  2. stirringstirring
  3. customthe mixture is evaporated down
  4. washThe ethyl acetate phase is washed with water
  5. customdried
  6. customevaporated down
  7. distillationDistillation

출처 및 근거

ORD 기록
ord-551240f347614c54874b79a1bb7ff07d
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659737

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