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4-Bromoaniline → N-(4-Bromophenyl)-3-oxobutanamide

HRID 734780
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HRID 734780 반응식
[CH2:1]=[C:2]1[O:6][C:4](=[O:5])[CH2:3]1.[Br:7][C:8]1[CH:14]=[CH:13][C:11]([NH2:12])=[CH:10][CH:9]=1>C1(C)C=CC=CC=1>[Br:7][C:8]1[CH:14]=[CH:13][C:11]([NH:12][C:4](=[O:5])[CH2:3][C:2](=[O:6])[CH3:1])=[CH:10][CH:9]=1
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참가 물질

4

반응물 2

HCID 78074-BromoanilineHCID 12661Diketene

생성물 1

HCID 598820N-(4-Bromophenyl)-3-oxobutanamide

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A solution of 25.72 mL (336 mmol) of diketene in 100 mL of toluene was added dropwise at 90° C. to a solution of 51.0 g (288 mmol) of 4-bromoaniline in 200 mL of toluene and the reaction mixture was kept at this temperature for 5 hours. The reaction solution was cooled in the ice bath, and the precipitate formed was filtered and washed with toluene until the product was virtually colorless. Subsequently it was dried at 50° C. in the circulating air dryer until a constant weight was obtained. Yield: 50.0 g (68% of theoretical); C10H10BrNO2 (M=256.096); calc.: molpeak (M+H)+: 256/258 (Br); found: molpeak (M+H)+: 256/258 (Br); HPLC-MS: 4.7 minutes (method B).

후처리

  1. customthe precipitate formed
  2. filtrationwas filtered
  3. washwashed with toluene until the product
  4. customSubsequently it was dried at 50° C. in the circulating air dryer until a constant weight
  5. customwas obtained
  6. custom4.7 minutes (method B)

출처 및 근거

ORD 기록
ord-6c3b42c3741f4d3b8268e01f62edd893
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07592358B2

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