Hydrogen Bromide → HCID 18756149, 화합물

HRID 433920노트

반응식

HRID 433920 반응식
[NH2:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:13])=[CH:7][CH:6]=1)(=[O:4])=[O:3].[BrH:20].BrBr>C(O)(=O)C>[NH2:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([CH:11]([Br:20])[C:12]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)=[O:13])=[CH:9][CH:10]=1)(=[O:3])=[O:4]

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 24408BromineHCID 222857924-(2-Oxo-2-phenylethyl)benzene-1-sulfonamide

생성물 1

HCID 18756149HCID 18756149, 화합물수율 80%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

To a mixture of 14.4 g (52 mmol) of 2-(4-aminosulfonylphenyl)-1-phenylethanone in 240 mL of glacial acetic acid stirred under nitrogen, a solution of 24 mL of hydrobromic acid in glacial acetic acid (33%) was added. To the reaction mixture was added slowly 8.4 g (52 mmol) of bromine. It was stirred at room temperature until complete loss of the colour. After concentration, the resulting residue was dissolved in ethyl acetate (500 mL). The organic layer was washed twice with 5% aqueous sodium bicarbonate solution (2×350 mL) and with brine (350 mL). The organic layer was dried, filtered and concentrated in vacuum. The residue was swished in hexane to give 14.9 g (80%) of the desired solid as a white powdered solid.

후처리

  1. stirringIt was stirred at room temperature until complete loss of the colour
  2. concentrationAfter concentration
  3. dissolutionthe resulting residue was dissolved in ethyl acetate (500 mL)
  4. washThe organic layer was washed twice with 5% aqueous sodium bicarbonate solution (2×350 mL) and with brine (350 mL)
  5. customThe organic layer was dried
  6. filtrationfiltered
  7. concentrationconcentrated in vacuum

출처 및 근거

ORD 기록
ord-d075e444edbd4641b8a3e85e9a16c4fb
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06670365B1

반응 노트

불러오는 중…