4-[(3-Hydroxypropyl)amino]-3-nitrobenzonitrile → 3-Amino-4-((3-hydroxypropyl)amino)benzonitrile

HRID 590407노트

반응식

HRID 590407 반응식
[OH:1][CH2:2][CH2:3][CH2:4][NH:5][C:6]1[CH:13]=[CH:12][C:9]([C:10]#[N:11])=[CH:8][C:7]=1[N+:14]([O-])=O>CCO>[NH2:14][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:6]=1[NH:5][CH2:4][CH2:3][CH2:2][OH:1])[C:10]#[N:11]

참가 물질

3

반응물 1

HCID 223493164-[(3-Hydroxypropyl)amino]-3-nitrobenzonitrile2회

생성물 1

HCID 223492773-Amino-4-((3-hydroxypropyl)amino)benzonitrile수율 100.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of 4-[(3-hydroxypropyl)amino]-3-nitrobenzonitrile (Intermediate 95, 13.4 g, 0.06 mol) in EtOH (500 mL) was added, under argon atmosphere, palladium over carbon (350 mg, 3.3 mmol of a 10% Pd/C) and the mixture was degassed. Then, H2 was added up to an internal pressure of 20 psi, and the final suspension was stirred at room temperature for 2.5 hours. The crude was filtered through a Whatmann glass micro fibre filter and the solvent was removed under reduced pressure to afford the title compound as a brownish solid (11.5 g, 95% yield) which was used in the next step without further purification.

후처리

  1. additionwas added, under argon atmosphere
  2. custompalladium over carbon (350 mg, 3.3 mmol of a 10% Pd/C) and the mixture was degassed
  3. additionThen, H2 was added up to an internal pressure of 20 psi
  4. filtrationThe crude was filtered through a Whatmann glass micro fibre
  5. filtrationfilter
  6. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-2dc2b9ecc0384d7f9da2111b2f260d93
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09233108B2

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