Trifluoroacetic acid → (2R, 5S)-2-[4-Chloro-2-(piperazine-1-carbonyl)-phenoxy]-1-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-ethanone

HRID 480183ノート

反応式

HRID 480183 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:42])[C:15]2[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:16]=2[O:22][CH2:23][C:24]([N:26]2[CH2:31][C@H:30]([CH3:32])[N:29]([CH2:33][C:34]3[CH:39]=[CH:38][C:37]([F:40])=[CH:36][CH:35]=3)[CH2:28][C@H:27]2[CH3:41])=[O:25])[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClC(Cl)C.ClCCl>[Cl:21][C:19]1[CH:18]=[CH:17][C:16]([O:22][CH2:23][C:24]([N:26]2[CH2:31][C@H:30]([CH3:32])[N:29]([CH2:33][C:34]3[CH:39]=[CH:38][C:37]([F:40])=[CH:36][CH:35]=3)[CH2:28][C@H:27]2[CH3:41])=[O:25])=[C:15]([C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)=[O:42])[CH:20]=1

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 12112117(2R, 5S)-4-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzoyl)-piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 9935847(2R, 5S)-2-[4-Chloro-2-(piperazine-1-carbonyl)-phenoxy]-1-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-ethanone収率 87.4%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 63651,1-Dichloroethane溶媒

実験手順

To a solution of (2R, 5S)-4-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzoyl)-piperazine-1-carboxylic acid tert-butyl ester (0.110 g, 0.182 mmol) in dichloroethane (10 ml) was added trifluoroacetic acid (5 ml). The reaction was stirred for two hours at ambient temperature. The reaction was then diluted with dichloromethane and washed with 1N aqueous sodium hydroxide. The organics were dried over magnesium sulfate, filtered and concentrated to give the title compound (0.080 g, 87% yield).

後処理

  1. washwashed with 1N aqueous sodium hydroxide
  2. dry with materialThe organics were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-1ef955aef3024dfbb6fac916cf1ca0e7
出典データセット
uspto-grants-2003_11
特許番号
US06649611B2

反応ノート

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