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

HRID 397061

反応式

HRID 397061 の反応式
[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]

参加物

3

反応物 1

HCID 86583958HCID 86583958、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

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)

後処理

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

出典と根拠

ORDレコード
ord-e2ab688b7a3f4015909250ff6dcb8c4d
出典データセット
uspto-grants-2003_08
特許番号
US06608203B2

関連ノート

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