Acetic Acid → Benzonitrile, 4-(5,6,7,8-tetrahydroimidazo(1,5-a)pyridin-5-yl)-, hydrochloride (1:1)

HRID 477965

反応式

HRID 477965 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]#[N:18])=[CH:13][CH:12]=2)[CH:8]=[N:7][CH:6]=1.CC(C)([O-])C.[K+].C(O)(=O)C>O1CCCC1.CC(C)=O.Cl>[ClH:1].[C:17]([C:14]1[CH:15]=[CH:16][C:11]([CH:10]2[N:9]3[CH:8]=[N:7][CH:6]=[C:5]3[CH2:4][CH2:3][CH2:2]2)=[CH:12][CH:13]=1)#[N:18]

参加物

7

反応物 3

HCID 176Acetic AcidHCID 136882095-(3-chloropropyl) 1-(p-cyanophenylmethyl)-1H-imidazoleHCID 23665647Potassium tert-butoxide

生成物 1

HCID 59694Benzonitrile, 4-(5,6,7,8-tetrahydroimidazo(1,5-a)pyridin-5-yl)-, hydrochloride (1:1)

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 313Hydrochloric Acid溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 8.1 g of 5-(3-chloropropyl) 1-(p-cyanophenylmethyl)-1H-imidazole in 50 ml of tetrahydrofuran is cooled to 0°. To this is added 7.0 g of potassium t-butoxide as a solid in portions. The mixture is stirred at room temperature for 2 h, neutralized with 10% acetic acid and partitioned between methylene chloride and water. The organic layer is washed with water, dried over magnesium sulfate and evaporated to yield an oil which is dissolved in a small volume of acetone and neutralized with ethereal hydrogen chloride. On cooling, the title compound is obtained as a white solid, m.p. 201°-203°.

後処理

  1. custompartitioned between methylene chloride and water
  2. washThe organic layer is washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customto yield an oil which
  6. temperatureOn cooling

出典と根拠

ORDレコード
ord-01fe519c295a477cbe06cf5746c0fa05
出典データセット
uspto-grants-1989_12
特許番号
US04889861

関連ノート

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