Benzoic acid, 3-(chlorosulfonyl)- → 3-{[[(3-Bromophenyl)methyl](methyl)amino]sulfonyl}benzoic acid

HRID 564567

반응식

HRID 564567 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][NH:9][CH3:10])[CH:5]=[CH:6][CH:7]=1.Cl[S:12]([C:15]1[CH:16]=[C:17]([CH:21]=[CH:22][CH:23]=1)[C:18]([OH:20])=[O:19])(=[O:14])=[O:13]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][N:9]([CH3:10])[S:12]([C:15]2[CH:16]=[C:17]([CH:21]=[CH:22][CH:23]=2)[C:18]([OH:20])=[O:19])(=[O:14])=[O:13])[CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 77641Benzoic acid, 3-(chlorosulfonyl)-HCID 457588Benzenemethanamine, 3-bromo-N-methyl-

생성물 1

HCID 578132513-{[[(3-Bromophenyl)methyl](methyl)amino]sulfonyl}benzoic acid수율 78.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-(3-Bromophenyl)-N-methylmethanamine (0.100 g, 0.5 mmol) in DCM (5 mL) was added TEA (0.139 mL, 1.000 mmol) and 3-(chlorosulfonyl)benzoic acid (0.110 g, 0.500 mmol). The resulting mixture was stirred at room temperature for 0.5 h. The reaction was quenched with HCl (1 N), concentrated and redissolved in EtOAc (10 mL) which was washed with H2O (2×3 mL), brine (3 mL), then dried with Na2SO4. It was then filtered and concentrated to afford the title compound (0.1505 g, 78%). LC-MS m/z 384 (M+H)+.

후처리

  1. customThe reaction was quenched with HCl (1 N)
  2. concentrationconcentrated
  3. dissolutionredissolved in EtOAc (10 mL) which
  4. washwas washed with H2O (2×3 mL), brine (3 mL)
  5. dry with materialdried with Na2SO4
  6. filtrationIt was then filtered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-caa4573a80e24f40a34fe6341b29b0f6
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067408B2

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