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Methanol → HCID 10413996、化合物

HRID 33598
ノート
印刷プレビュー

反応式

HRID 33598 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 10413996HCID 10413996、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8471Triethylamine
溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f87b85ae63044e2580b8bd74139cf8b7
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07429612B2

反応ノート

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