Water → (1-(fur-3-ylmethyl)-1H-benzimidazol-2-yl)(piperidin-4-yl)amine

HRID 323487ノート

反応式

HRID 323487 の反応式
[O:1]1[CH:5]=[CH:4][C:3]([CH2:6][N:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[NH:16][CH:17]2[CH2:22][CH2:21][N:20](C(OCC)=O)[CH2:19][CH2:18]2)=[CH:2]1.[OH-].[K+].O>C(O)(C)C.O>[O:1]1[CH:5]=[CH:4][C:3]([CH2:6][N:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[NH:16][CH:17]2[CH2:18][CH2:19][NH:20][CH2:21][CH2:22]2)=[CH:2]1

参加物

6

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 13587984HCID 13587984、化合物

生成物 1

HCID 22009357(1-(fur-3-ylmethyl)-1H-benzimidazol-2-yl)(piperidin-4-yl)amine

試薬・触媒・溶媒 2

HCID 962Water触媒HCID 3776Isopropanol溶媒

実験手順

Combine (1-(fur-3-ylmethyl)-1H-benzimidazol-2-yl)(1-(ethoxycarbonyl)piperidin-4-yl)amine (0.98 g, 2.67 mmol), potassium hydroxide (1.8 g, 32 mmol) in isopropanol (18 mL) containing 1 drop of water. Heat to reflux. After 18 hours, cool, add water, and extract four times with dichloromethane (200 mL). Combine the organic layers, dry over MgSO4, filter, and concentrate in vacuo to give the title compound: Rf=0.40 (silica gel, ethyl acetate).

後処理

  1. temperatureHeat to reflux
  2. temperaturecool
  3. extractionextract four times with dichloromethane (200 mL)
  4. dry with materialCombine the organic layers, dry over MgSO4
  5. filtrationfilter
  6. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-65209075db374a14b77e38337c42baa8
出典データセット
uspto-grants-2001_04
特許番号
US06211199B1

反応ノート

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