2-Bromo-4-nitro-1-(propan-2-yl)benzene → 3-Bromo-4-isopropylaniline

HRID 59584

반응식

HRID 59584 반응식
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][C:3]=1[CH:11]([CH3:13])[CH3:12]>[Pt].[Br-].[Br-].[Zn+2].CO>[Br:1][C:2]1[CH:7]=[C:6]([CH:5]=[CH:4][C:3]=1[CH:11]([CH3:13])[CH3:12])[NH2:8]

참가 물질

5

반응물 1

HCID 215316212-Bromo-4-nitro-1-(propan-2-yl)benzene

생성물 1

HCID 2807993-Bromo-4-isopropylaniline수율 104.1%

시약·촉매·용매 3

HCID 23939Platinum촉매HCID 10421208Zinc bromide촉매HCID 887Methanol용매

실험 절차

2-Bromo-1-isopropyl-4-nitrobenzene (XI) (20 g, 78.1 mmol, 95.8 GC % by area), methanol (400 ml), platinum on carbon (5% of platinum, poisoned with sulphur, moist with water) (1.0 g, 0.090 mmol) and zinc dibromide (265 mg, 1.18 mmol) were placed in a 600 ml autoclave. The autoclave was subsequently flushed with nitrogen and pressurized to 5 bar with hydrogen at room temperature. The contents of the autoclave were filtered through Celite, washed with methanol and the solvent was distilled off under reduced pressure. 3-Bromo-4-isopropylaniline (17.4 g, 94.5 LC-% by area, 97.7 GC-% by area, >99% of theory) was obtained as a brown oil.

후처리

  1. customThe autoclave was subsequently flushed with nitrogen
  2. custompressurized to 5 bar with hydrogen at room temperature
  3. filtrationThe contents of the autoclave were filtered through Celite
  4. washwashed with methanol
  5. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-532af21f19f842208c8ea50eafe144de
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440908B2

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