1,1'-Carbonyldiimidazole → HCID 59333745、化合物

HRID 1930725

反応式

HRID 1930725 の反応式
N1([C:6]([N:8]2[CH:12]=[CH:11][N:10]=[CH:9]2)=[O:7])C=CN=C1.[O:13]1[CH2:17][CH2:16][CH2:15][CH:14]1[CH2:18][CH2:19]C(O)=O>ClCCl>[N:8]1([C:6](=[O:7])[CH2:19][CH2:18][CH:14]2[CH2:15][CH2:16][CH2:17][O:13]2)[CH:12]=[CH:11][N:10]=[CH:9]1

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 2631613-(Oxolan-2-yl)propanoic acid

生成物 1

HCID 59333745HCID 59333745、化合物収率 81%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Di(1H-imidazol-1-yl)methanone (1.196 g, 7.38 mmol) was added in small portions to a stirred solution of 3-(tetrahydrofuran-2-yl)propanoic acid (1.013 g, 7.03 mmol) in dichloromethane (3 mL) at room temperature under argon. The reaction mixture was stirred at room temperature for 2 hours. The mixture was washed twice with water, dried over MgSO4 and concentrated giving 1-(1H-imidazol-1-yl)-3-(tetrahydrofuran-2-yl)propan-1-one (1.099 g, 81%) as the product. 1H NMR (500 MHz, DMSO-d6) δ ppm 8.34-8.51 (m, 1 H), 7.64-7.79 (m, 1 H), 6.98-7.17 (m, 1 H), 3.76-3.85 (m, 1 H), 3.66-3.76 (m, 1 H), 3.55-3.60 (m, 1 H), 3.03-3.10 (m, 2 H), 1.90-2.00 (m, 1 H), 1.73-1.90 (m, 4 H), 1.39-1.53 (m, 1 H); MS (ES−) m/z 194 (M−H)−.

後処理

  1. washThe mixture was washed twice with water
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-c3ed194a9765471ca829d3e3253a8f90
出典データセット
uspto-grants-2012_05
特許番号
US08188101B2

関連ノート

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