Hydrochloric Acid → HCID 20030105、化合物

HRID 638004ノート

反応式

HRID 638004 の反応式
[C:1]([CH2:3][N:4]1[CH2:9][CH2:8][CH:7]([C:10](=[O:18])[C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)[CH2:6][CH2:5]1)#[N:2].[ClH:19].[H][H]>C(O)(=O)C.[Pt]=O>[ClH:19].[NH2:2][CH2:1][CH2:3][N:4]1[CH2:5][CH2:6][CH:7]([C:10](=[O:18])[C:11]2[CH:12]=[CH:13][C:14]([F:17])=[CH:15][CH:16]=2)[CH2:8][CH2:9]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 30200424-(4-Fluorobenzoyl)piperidine-1-acetonitrileHCID 178418361HCID 178418361、化合物

生成物 1

HCID 20030105HCID 20030105、化合物

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 176Acetic Acid溶媒

実験手順

14.1 g (0.05 mol) of N-(cyanomethyl)-4-(p-fluorobenzoyl)-piperidine are dissolved in 1.5 liters of glacial acetic acid and 30 ml of concentrated hydrochloric acid and hydrogenated together with 2 g of platinum oxide in a hydrogen atmosphere. After 6 hours, the theoretical amount of 2.25 liters of hydrogen is absorbed. The catalyst is then filtered off with suction and the filtrate is concentrated to approximately 30 ml in a water-jet vacuum. There is added to the resulting crystal mass 5 ml of isopropanol and 15 ml of ether and filtration with suction is carried out. After filtration with suction and drying, N-(2-aminoethyl)-4-(p-fluorobenzoyl)-piperidine hydrochloride is obtained which, after recrystallisation from methanol, melts at 265° with decomposition.

後処理

  1. customthe theoretical amount of 2.25 liters of hydrogen is absorbed
  2. filtrationThe catalyst is then filtered off with suction
  3. concentrationthe filtrate is concentrated to approximately 30 ml in a water-jet vacuum
  4. additionThere is added to the resulting crystal mass 5 ml of isopropanol and 15 ml of ether and filtration with suction
  5. filtrationAfter filtration with suction
  6. customdrying

出典と根拠

ORDレコード
ord-d88d9fd90de44b5fae36cb4b229aa33d
出典データセット
uspto-grants-1985_12
特許番号
US04559349

反応ノート

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