Benzenamine, N-propyl- → 1-Phenyl-1-propylhydrazine

HRID 127958

반응식

HRID 127958 반응식
[N:1]([N:3]([CH2:10][CH2:11][CH3:12])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=O.C(NC1C=CC=CC=1)CC.[H-].[Al+3].[Li+].[H-].[H-].[H-]>CCOCC>[C:4]1([N:3]([CH2:10][CH2:11][CH3:12])[NH2:1])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 12153Benzenamine, N-propyl-HCID 12937302N-Phenyl-N-propylnitrous amideHCID 21226445Aluminium lithium hydride2회

생성물 1

HCID 123271621-Phenyl-1-propylhydrazine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

N-nitroso-N-propylaniline, prepared from N-n-propylaniline by the same method as described in Example 1, was conveniently reduced with lithium aluminum hydride (LAH). The LAH in 450 ml dry ether was heated under reflux for 15 minutes, and a solution of 32.8 g (0.2 mol) crude 4 in 250 ml dry ether was added dropwise. The reaction mixture was allowed to stir for 3 hours before it was quenched by the dropwise addition of 12 ml water and 14 ml 20% sodium hydroxide. The resultant suspension was filtered free of inorganic salts, dried and stripped of solvents under diminished pressure. Distillation of the residue yielded the desired compound bp 55°-57°/0.12 mm.

후처리

  1. temperatureunder reflux for 15 minutes
  2. customwas quenched by the dropwise addition of 12 ml water and 14 ml 20% sodium hydroxide
  3. filtrationThe resultant suspension was filtered free of inorganic salts
  4. customdried
  5. distillationDistillation of the residue

출처 및 근거

ORD 기록
ord-207580a4e11c40449621047bd2f67b3a
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04258059

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