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Dimethylamine tetrahydrofuran → Benzo[b]thiophene-2-sulfonic acid {2-[5-(2-dimethylaminoethanesulfonyl)-2-methoxybenzenesulfonylamino]phenyl}-amide

HRID 730224
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HRID 730224 반응식
[CH:1]([S:3]([C:6]1[CH:7]=[CH:8][C:9]([O:35][CH3:36])=[C:10]([S:12]([NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[NH:22][S:23]([C:26]2[S:30][C:29]3[CH:31]=[CH:32][CH:33]=[CH:34][C:28]=3[CH:27]=2)(=[O:25])=[O:24])(=[O:14])=[O:13])[CH:11]=1)(=[O:5])=[O:4])=[CH2:2].[NH:37]([CH3:39])[CH3:38].C1COCC1>C1COCC1>[CH3:38][N:37]([CH3:39])[CH2:2][CH2:1][S:3]([C:6]1[CH:7]=[CH:8][C:9]([O:35][CH3:36])=[C:10]([S:12]([NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[NH:22][S:23]([C:26]2[S:30][C:29]3[CH:31]=[CH:32][CH:33]=[CH:34][C:28]=3[CH:27]=2)(=[O:25])=[O:24])(=[O:13])=[O:14])[CH:11]=1)(=[O:4])=[O:5]
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참가 물질

4

반응물 2

HCID 22320367Dimethylamine tetrahydrofuranHCID 86605045Benzo[b]thiophene-2-sulfonic acid [2-(5-ethenesulfonyl-2-methoxybenzenesulfonylamino)phenyl] amide

생성물 1

HCID 11678864Benzo[b]thiophene-2-sulfonic acid {2-[5-(2-dimethylaminoethanesulfonyl)-2-methoxybenzenesulfonylamino]phenyl}-amide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of benzo[b]thiophene-2-sulfonic acid [2-(5-ethenesulfonyl-2-methoxy-benzenesulfonylamino) -phenyl]-amide (0.5 mmol), as prepared above, in dry THF (10 mL), Me2NH-THF solution (2.5 mL; 2 M Me2NH in THF solution) was added. The resulting reaction mixture was stirred at room temperature for 30 min. After removal of the solvent under vacuum, the residue obtained was purified by flash column chromatography eluting with EtOAc then DCM/methanol (100:2 to 100:10) to give 290 mg of benzo[b]thiophene-2-sulfonic acid {2-[5-(2-dimethylaminoethanesulfonyl)-2-methoxybenzenesulfonylamino]phenyl}-amide. LC: Tr 0.99 min; MS: 610.7 (M+1)+.

후처리

  1. customThe resulting reaction mixture
  2. customAfter removal of the solvent under vacuum
  3. customthe residue obtained
  4. customwas purified by flash column chromatography
  5. washeluting with EtOAc

출처 및 근거

ORD 기록
ord-4bba2c06ef334f149056f83e7824d33b
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582673B2

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