Pyridine → Ethyl 4-benzyl-2-(trifluoromethyl)piperazine-1-carboxylate

HRID 2067887ノート

反応式

HRID 2067887 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][NH:11][CH:10]([C:14]([F:17])([F:16])[F:15])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N1C=CC=CC=1.Cl[C:25]([O:27][CH2:28][CH3:29])=[O:26]>C(Cl)Cl>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH:10]([C:14]([F:17])([F:15])[F:16])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 10928Ethyl chloroformateHCID 534071701-Benzyl-3-(trifluoromethyl)piperazine

生成物 1

HCID 68748441Ethyl 4-benzyl-2-(trifluoromethyl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 1-benzyl-3-(trifluoromethyl)piperazine 34a (1.0 mmol) and pyridine (1.1 mmol) in DCM (5 mL), is added ethyl chloroformate (1.1 mmol). The resulting mixture is stirred at rt for 1 h. After the reaction is complete, the reaction mixture is diluted with DCM (15 mL) and washed with water. The organic layer is separated, dried over Na2SO4, filtered, and concentrated to afford ethyl 4-benzyl-2-(trifluoromethyl)piperazine-1-carboxylate 34b, which is used without purification. MS (m/z) (M+1)+: 317.1.

後処理

  1. washwashed with water
  2. customThe organic layer is separated
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-905d12cf53f54e80aecdd4a690d6e656
出典データセット
uspto-grants-2012_10
特許番号
US08293757B2

反応ノート

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