HCID 86583958, 화합물 → 2,2,2-Trifluoro-1-[4-(6-methoxy-3,4-dihydro-isoquinolin-1-yl)-piperidin-1-yl]-ethanone

HRID 397061노트

반응식

HRID 397061 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][NH:11][C:12]([CH:14]2[CH2:19][CH2:18][N:17]([C:20](=[O:25])[C:21]([F:24])([F:23])[F:22])[CH2:16][CH2:15]2)=O)[CH:6]=[CH:7][CH:8]=1>O=P(Cl)(Cl)Cl>[F:22][C:21]([F:24])([F:23])[C:20]([N:17]1[CH2:18][CH2:19][CH:14]([C:12]2[C:6]3[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=3)[CH2:9][CH2:10][N:11]=2)[CH2:15][CH2:16]1)=[O:25]

참가 물질

3

반응물 1

HCID 86583958HCID 86583958, 화합물

생성물 1

HCID 181723932,2,2-Trifluoro-1-[4-(6-methoxy-3,4-dihydro-isoquinolin-1-yl)-piperidin-1-yl]-ethanone수율 88.3%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

A stirred solution of 1-trifluoroacetyl-piperidine-4-carboxylic acid [2-(3-methoxy-phenyl)-ethyl]-amide (1.04 g, 2.9 mmol) in POCl3 under an atmosphere of N2 was heated at reflux for 2.5 hours. The reaction was allowed to cool to RT and the POCl3 was removed in vacuo. The residual oil was suspended in toluene (20 ml) and concentrated in vacuo (this process was repeated twice more), leaving the desired product as a tan colored solid (0.872 g, 2.56 mmol, 88% yield). MS 341 (M+1)

후처리

  1. temperatureat reflux for 2.5 hours
  2. customthe POCl3 was removed in vacuo
  3. concentrationconcentrated in vacuo (this process

출처 및 근거

ORD 기록
ord-e2ab688b7a3f4015909250ff6dcb8c4d
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06608203B2

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