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alpha,alpha,alpha',alpha'-Tetramethyl-1,3-benzenedipropionitrile → 1,3-Bis(2,2-dimethyl-3-aminopropyl)benzene

HRID 544765
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HRID 544765 반응식
[CH3:1][C:2]([C:17]#[N:18])([CH3:16])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH2:10][C:11]([C:14]#[N:15])([CH3:13])[CH3:12])[CH:5]=1.[H-].C([Al+]CC(C)C)C(C)C>C1(C)C=CC=CC=1>[CH3:12][C:11]([CH3:13])([CH2:14][NH2:15])[CH2:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([CH2:3][C:2]([CH3:1])([CH3:16])[CH2:17][NH2:18])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 13587560alpha,alpha,alpha',alpha'-Tetramethyl-1,3-benzenedipropionitrileHCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 135875571,3-Bis(2,2-dimethyl-3-aminopropyl)benzene

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

In a 1-liter flask equipped with a paddle stirrer, a reflux condenser capped with a nitrogen bubbler, and an addition funnel, was placed 7.50 g of 1,3-bis(2-methyl-2-cyanopropyl)benzene and 250 ml of reagent grade toluene which had been passed through acid alumina under nitrogen directly into the reaction vessel. With stirring at room temperature, 107 ml of a 25% solution of diisobutylaluminum hydride in toluene was added in 1 hr. The mixture was refluxed for 17 hrs 15 min. The mixture was then worked up as described in Example 1(b). Upon distillation of the isolated product through a small Vigreux still, there was otained 3.51 g of 1,3-bis(2,2-dimethyl-3-aminopropyl)benzene as a colorless liquid distilling at 105° to 110°/0.05 mm.

후처리

  1. customIn a 1-liter flask equipped with a paddle stirrer, a reflux condenser
  2. customcapped with a nitrogen bubbler, and an addition funnel
  3. temperatureThe mixture was refluxed for 17 hrs 15 min
  4. distillationUpon distillation of the isolated product through a small Vigreux still
  5. distillationdistilling at 105° to 110°/0.05 mm

출처 및 근거

ORD 기록
ord-f420d6e97cf847b38c8a7137543cb525
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04451642

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