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Water → HCID 15579464, 화합물

HRID 2166218
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HRID 2166218 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 (0.1M) 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 (0.1M) 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 methanol-water 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 methanol-water 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-1ba38b8606634a5390d4ec26fefc4d2c
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04943655

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