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Methanol → HCID 10413996, 화합물

HRID 33598
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HRID 33598 반응식
[CH3:1][OH:2].Cl[S:4]([N:7]=[C:8]=[O:9])(=[O:6])=[O:5].[NH2:10][C:11]1[C:12]([CH3:36])=[C:13]2[C:17](=[C:18]([NH:21][C:22](=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24])[C:19]=1[CH3:20])[N:16]([CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])[CH2:15][CH2:14]2>C(Cl)Cl.C(N(CC)CC)C>[CH3:1][O:2][C:8]([NH:7][S:4]([NH:10][C:11]1[C:12]([CH3:36])=[C:13]2[C:17](=[C:18]([NH:21][C:22](=[O:27])[C:23]([CH3:25])([CH3:26])[CH3:24])[C:19]=1[CH3:20])[N:16]([CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])[CH2:15][CH2:14]2)(=[O:6])=[O:5])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 887MethanolHCID 70918Chlorosulfonyl isocyanateHCID 23075425N-(5-Amino-4,6-dimethyl-1-octylindolin-7-yl)-2,2-dimethylpropanamide

생성물 1

HCID 10413996HCID 10413996, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 8471Triethylamine
용매

실험 절차

Methanol (0.13 mL) was added to methylene chloride (2.6 mL) and chlorosulfonyl isocyanate (0.29 mL) was added at −20° C. The mixture was stirred at −20° C. to 10° C. for 20 min. N-(5-Amino-4,6-dimethyl-1-octylindolin-7-yl)-2,2-dimethylpropanamide (612 mg) and triethylamine (0.46 mL) were added to the reaction mixture and the mixture was further stirred at −9° C. for 30 min. Methylene chloride was added to the reaction mixture, and the mixture was washed successively with 10% aqueous citric acid, saturated aqueous sodium hydrogencarbonate and saturated brine and dried over sodium sulfate. Methylene chloride was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as crystals. (601 mg).

후처리

  1. additionwas added at −20° C
  2. stirringthe mixture was further stirred at −9° C. for 30 min
  3. washthe mixture was washed successively with 10% aqueous citric acid, saturated aqueous sodium hydrogencarbonate and saturated brine
  4. dry with materialdried over sodium sulfate
  5. customMethylene chloride was evaporated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-f87b85ae63044e2580b8bd74139cf8b7
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07429612B2

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