Triethylamine → HCID 11419234、化合物

HRID 748070ノート

反応式

HRID 748070 の反応式
[CH2:1]([N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[CH:13]([NH2:19])[CH:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[Cl:27][C:28]1[S:32][C:31]([S:33](Cl)(=[O:35])=[O:34])=[CH:30][CH:29]=1>C(Cl)Cl.CCOC(C)=O>[CH2:1]([N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[CH:13]([NH:19][S:33]([C:31]1[S:32][C:28]([Cl:27])=[CH:29][CH:30]=1)(=[O:35])=[O:34])[CH:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 27339255-Chlorothiophene-2-sulfonyl chlorideHCID 68593891HCID 68593891、化合物

生成物 1

HCID 11419234HCID 11419234、化合物収率 59%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a stirred solution of [1-(1-benzyl-1H-imidazol-2-yl)-2-ethylbutyl]amine (448 mg, 1.74 mmol) in CH2Cl2 (15 mL) was added triethylamine (0.36 mL, 2.6 mmol) and 5-chlorothiophene-2-sulfonylchloride (453 mg, 2.09 mmol). The mixture was stirred for 3.5 h and then diluted with EtOAc, washed twice with 1N HCl, dried over MgSO4, filtered and concentrated in vacuo. The resulting oil was purified by column chromatography (SiO2, CHCl3, then 1% MeOH/CHCl3 to 2% MeOH/CHCl3) to yield a white solid in 59% yield.

後処理

  1. washwashed twice with 1N HCl
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe resulting oil was purified by column chromatography (SiO2, CHCl3
  6. custom1% MeOH/CHCl3 to 2% MeOH/CHCl3) to yield a white solid in 59% yield

出典と根拠

ORDレコード
ord-d5227f5e731b4d78ab014ec72be50233
出典データセット
uspto-grants-2008_07
特許番号
US07399778B2

反応ノート

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