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Water → HCID 15579464, 화합물

HRID 1721832
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HRID 1721832 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([CH3:14])=[C:8]([S:10]([NH2:13])(=[O:12])=[O:11])[CH:9]=1)(=[O:3])[CH3:2].[Br:15]Br.O>CO>[Br:15][CH2:2][C:1]([C:4]1[CH:5]=[CH:6][C:7]([CH3:14])=[C:8]([S:10]([NH2:13])(=[O:11])=[O:12])[CH:9]=1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24408BromineHCID 126197975-Acetyl-2-methylbenzene-1-sulfonamide

생성물 1

HCID 15579464HCID 15579464, 화합물수율 95.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

21.3 Grams (0.1 M) of 5-acetyl-2-methylbenzenesulfonamide was dissolved in 180 g of methanol, while the resulting solution was kept at 35°-40° C., 16.0 g (0.1 M) of bromine was added dropwise by taking 1.5 hours. The reaction mixture was stirred for 10 minutes after the dropwise addition, 80 g of water was added to the reaction mixture and the whole reaction mixture was stirred for further 30 minutes at room temperature. A part of methanolwater was removed by evaporation, then the crystals formed were collected by filtration, washed with water and dried to obtain 28.0 g of 5-bromoacetyl-2-methylbenzenesulfonamide in the form of white crystals. Melting point: 146.5°-147.5° C Yield: 95.9%.

후처리

  1. customwas kept at 35°-40° C.
  2. additionwas added to the reaction mixture
  3. customthe whole reaction mixture
  4. stirringwas stirred for further 30 minutes at room temperature
  5. customA part of methanolwater was removed by evaporation
  6. customthe crystals formed
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customdried

출처 및 근거

ORD 기록
ord-ca5f3c63e82349399f3fc79049391fe8
출처 데이터셋
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04853158

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