Hydrochloric Acid → HCID 20030105, 화합물

HRID 638004노트

반응식

HRID 638004 반응식
[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

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 30200424-(4-Fluorobenzoyl)piperidine-1-acetonitrileHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 20030105HCID 20030105, 화합물

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d88d9fd90de44b5fae36cb4b229aa33d
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04559349

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