Methanesulfonyl chloride → HCID 70223394, 화합물

HRID 1531554노트

반응식

HRID 1531554 반응식
[C:1]([O:5][C:6](=[O:45])[N:7]([CH2:23][CH2:24][C:25]1[C:33]2[C:28](=[CH:29][CH:30]=[C:31]([N+:34]([O-:36])=[O:35])[CH:32]=2)[NH:27][C:26]=1[C:37]1[CH:42]=[C:41]([CH3:43])[CH:40]=[C:39]([CH3:44])[CH:38]=1)[CH2:8][CH2:9][CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([NH:18]S(C)(=O)=O)=[CH:14][CH:13]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:46][S:47](Cl)(=[O:49])=[O:48]>C(N(CC)CC)C>[C:1]([O:5][C:6](=[O:45])[N:7]([CH2:23][CH2:24][C:25]1[C:33]2[C:28](=[CH:29][CH:30]=[C:31]([N+:34]([O-:36])=[O:35])[CH:32]=2)[NH:27][C:26]=1[C:37]1[CH:38]=[C:39]([CH3:44])[CH:40]=[C:41]([CH3:43])[CH:42]=1)[CH2:8][CH2:9][CH2:10][CH2:11][C:12]1[CH:13]=[CH:14][C:15]([NH2:18])=[C:16]([S:47]([CH3:46])(=[O:49])=[O:48])[C:17]=1[S:47]([CH3:46])(=[O:49])=[O:48])([CH3:2])([CH3:4])[CH3:3]

참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 54430957HCID 54430957, 화합물

생성물 1

HCID 70223394HCID 70223394, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To a solution of {2-[2-(3,5-dimethylphenyl)-5-nitro-1H-indol-3-yl]ethyl}-[4-(4-methanesulfonylaminophenyl)butyl]carbamic acid tert-butyl ester (300 mg in 7 mL methylene chloride) at 0° C. was added 0.135 mL triethylamine and 0.066 mL methanesulfonyl chloride and the mixture sired at low temperature. After 30 minutes, the reaction was quenched by the addition of saturated aqueous sodium bicarbonate and partitioned between water and ethyl acetate. The organic portion was washed successively with saturated ammonium chloride, saturated sodium bicarbonate and brine, then dried over sodium sulfate and concentrated in vacuo to give the crude title compound (330 mg).

후처리

  1. customthe reaction was quenched by the addition of saturated aqueous sodium bicarbonate
  2. custompartitioned between water and ethyl acetate
  3. washThe organic portion was washed successively with saturated ammonium chloride, saturated sodium bicarbonate and brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0078c30df14342ed8046e3ca6b49f495
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06197975B1

반응 노트

불러오는 중…