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5-Chloro-3-methylbenzo(b)thiophene-2-sulfonyl chloride → HCID 18180112, 화합물

HRID 2230135
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HRID 2230135 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH2:16])[CH:6]=[CH:7][C:8]=1[N:9]1[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]1.[Cl:17][C:18]1[CH:31]=[CH:30][C:21]2[S:22][C:23]([S:26](Cl)(=[O:28])=[O:27])=[C:24]([CH3:25])[C:20]=2[CH:19]=1>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:16][S:26]([C:23]2[S:22][C:21]3[CH:30]=[CH:31][C:18]([Cl:17])=[CH:19][C:20]=3[C:24]=2[CH3:25])(=[O:28])=[O:27])[CH:6]=[CH:7][C:8]=1[N:9]1[CH2:10][CH2:11][N:12]([CH3:15])[CH2:13][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 27357565-Chloro-3-methylbenzo(b)thiophene-2-sulfonyl chlorideHCID 118447613-Methoxy-4-(4-methylpiperazin-1-yl)aniline

생성물 1

HCID 18180112HCID 18180112, 화합물수율 34%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 3-methoxy-4-(4-methylpiperazin-1-yl)phenylamine (D35) (50 mg, 0.23 mmol) and 5-chloro-3-methylbenzo[b]thiophene-2-sulfonyl chloride (64 mg, 0.23 mmol) in dichloromethane (2 ml) was allowed to stand at room temperature overnight. The reaction mixture was diluted with dichloromethane and washed with potassium carbonate (aq), which was back-extracted with further dichloromethane. The combined organic phases were dried (Na2SO4) and evaporated under reduced pressure to give a crude product, which was purified by chromatography on silica gel, eluting with methanol and dichloromethane. This gave the title compound (E128) as an off-white solid (36 mg, 34%) MH+=466.

후처리

  1. washwashed with potassium carbonate (aq), which
  2. extractionwas back-extracted with further dichloromethane
  3. dry with materialThe combined organic phases were dried (Na2SO4)
  4. customevaporated under reduced pressure
  5. customto give a crude product, which
  6. customwas purified by chromatography on silica gel
  7. washeluting with methanol and dichloromethane

출처 및 근거

ORD 기록
ord-125e53b526214c88b7b74850ac0275bb
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06423717B1

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