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Triethylamine → 7-Oxo-4,5,6,7-tetrahydro-benzo[b]thiophene-3-sulfonic acid [2-(4-fluorophenyl)-ethyl]-methyl-amide

HRID 1351269
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HRID 1351269 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][NH:10][CH3:11])=[CH:4][CH:3]=1.C(N(CC)CC)C.[O:19]=[C:20]1[C:25]2[S:26][CH:27]=[C:28]([S:29](Cl)(=[O:31])=[O:30])[C:24]=2[CH2:23][CH2:22][CH2:21]1>O1CCCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][N:10]([CH3:11])[S:29]([C:28]2[C:24]3[CH2:23][CH2:22][CH2:21][C:20](=[O:19])[C:25]=3[S:26][CH:27]=2)(=[O:30])=[O:31])=[CH:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 120234(2-(4-Fluorophenyl)ethyl)(methyl)amineHCID 210986857-Oxo-4,5,6,7-tetrahydrobenzo[b]thiophene-3-sulfonyl chloride

생성물 1

HCID 866009897-Oxo-4,5,6,7-tetrahydro-benzo[b]thiophene-3-sulfonic acid [2-(4-fluorophenyl)-ethyl]-methyl-amide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of [2-(4-fluorophenyl)-ethyl]-methyl-amine (the compound of Preparation Example 14) (520 mg) and triethylamine (474 μL) in tetrahydrofuran was added a solution of 7-oxo-4,5,6,7-tetrahydro-benzo[b]thiophene-3-sulfonyl chloride (the compound of Preparation Example 7) (800 mg) in tetrahydrofuran. The solution was stirred on an ice bath for 30 minutes, and at room temperature for 30 minutes. The residue resulting from the removal of the solvent by evaporation was purified by NH silica gel column chromatography (hexane/ethyl acetate), and the title compound (834 mg) was obtained as a colorless candy-like substance.

후처리

  1. waitat room temperature for 30 minutes
  2. customThe residue resulting from the removal of the solvent by evaporation
  3. customwas purified by NH silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-6659fbf53375402481e1cc594238ba74
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07217723B2

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