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

HRID 1023349노트

반응식

HRID 1023349 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-dbde279ecdb747d1a9b879cd89001f0f
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722663B2

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