Trifluoroacetic acid → 1-(4-Diisopropylaminomethylbenzoyl)piperazine

HRID 278549ノート

反応式

HRID 278549 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:29])[C:15]2[CH:20]=[CH:19][C:18]([CH2:21][N:22]([CH:26]([CH3:28])[CH3:27])[CH:23]([CH3:25])[CH3:24])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(OCC)(=O)C>[CH:23]([N:22]([CH2:21][C:18]1[CH:19]=[CH:20][C:15]([C:14]([N:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[O:29])=[CH:16][CH:17]=1)[CH:26]([CH3:28])[CH3:27])([CH3:24])[CH3:25]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 226280611-(Tert-butoxycarbonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine

生成物 1

HCID 226279521-(4-Diisopropylaminomethylbenzoyl)piperazine収率 90.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-(tert-butoxycarbonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine (4.6 g) in ethyl acetate (10 ml) was added trifluoroacetic acid (20 ml), and the solution was stirred at room temperature for 1 hour and concentrated. The residue was dissolved in water. The solution was made alkaline with sodium hydroxide solution, extracted with dichloromethane. The extract was dried and concentrated to give amorphous powders which were filtered, washed with hexane and dried to afford the title compound (3.12 g).

後処理

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in water
  3. extractionextracted with dichloromethane
  4. customThe extract was dried
  5. concentrationconcentrated
  6. customto give amorphous powders which
  7. filtrationwere filtered
  8. washwashed with hexane
  9. customdried

出典と根拠

ORDレコード
ord-084ef76c38a54aa4b696a7f2a3824efa
出典データセット
uspto-grants-2002_03
特許番号
US06359134B1

反応ノート

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