Trifluoroacetic acid → 1-(4-{[4-(Propan-2-yloxy)phenoxy]methyl}benzyl)piperazine

HRID 1023349ノート

反応式

HRID 1023349 の反応式
[CH3:1][CH:2]([O:4][C:5]1[CH:32]=[CH:31][C:8]([O:9][CH2:10][C:11]2[CH:30]=[CH:29][C:14]([CH2:15][N:16]3[CH2:21][CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18][CH2:17]3)=[CH:13][CH:12]=2)=[CH:7][CH:6]=1)[CH3:3].C(O)(C(F)(F)F)=O.[OH-].[Na+]>C(Cl)Cl>[CH3:3][CH:2]([O:4][C:5]1[CH:32]=[CH:31][C:8]([O:9][CH2:10][C:11]2[CH:30]=[CH:29][C:14]([CH2:15][N:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)=[CH:13][CH:12]=2)=[CH:7][CH:6]=1)[CH3:1]

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 67328500Tert-butyl 4-(4-{[4-(propan-2-yloxy)phenoxy]methyl}benzyl)piperazine-1-carboxylate

生成物 1

HCID 673276971-(4-{[4-(Propan-2-yloxy)phenoxy]methyl}benzyl)piperazine収率 136.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl 4-(4-{[4-(propan-2-yloxy)phenoxy]methyl}benzyl)-piperazine-1-carboxylate (5.42 g) in CH2Cl2 (41 mL) was added TFA (10 mL) at room temperature, then the reaction mixture was stirred for 8 hours. The reaction mixture was basified with 5 M aqueous NaOH, and extracted with CH2Cl2. The organic layer was washed with water and saturated aqueous NaCl, dried over anhydrous Na2SO4, and concentrated under reduced pressure to afford 1-(4-{[4-(propan-2-yloxy)phenoxy]methyl}benzyl)piperazine as a colorless solid (5.73 g).

後処理

  1. extractionextracted with CH2Cl2
  2. washThe organic layer was washed with water and saturated aqueous NaCl
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-dbde279ecdb747d1a9b879cd89001f0f
出典データセット
uspto-grants-2014_05
特許番号
US08722663B2

反応ノート

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