Trifluoroacetic acid → Methyl 4-({2-[2-(4-bromobenzyloxy)phenyl]ethylamino}methyl)benzoate

HRID 1672611

반응식

HRID 1672611 반응식
[Br:1][C:2]1[CH:36]=[CH:35][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[CH2:14][CH2:15][N:16]([CH2:24][C:25]2[CH:34]=[CH:33][C:28]([C:29]([O:31][CH3:32])=[O:30])=[CH:27][CH:26]=2)C(OC(C)(C)C)=O)=[CH:4][CH:3]=1.FC(F)(F)C(O)=O.C(=O)(O)[O-].[Na+]>ClCCl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[CH2:14][CH2:15][NH:16][CH2:24][C:25]2[CH:26]=[CH:27][C:28]([C:29]([O:31][CH3:32])=[O:30])=[CH:33][CH:34]=2)=[CH:35][CH:36]=1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 57864402Methyl 4-[({2-[2-(4-bromobenzyloxy)phenyl]ethyl}-tert-butoxycarbonylamino)methyl]benzoate

생성물 1

HCID 22014995Methyl 4-({2-[2-(4-bromobenzyloxy)phenyl]ethylamino}methyl)benzoate수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 4.2 g (7.57 mmol) of methyl 4-[({2-[2-(4-bromobenzyloxy)phenyl]ethyl}-tert-butoxycarbonylamino)methyl]benzoate from Example 4A in 15 ml of dichloromethane is stirred with 15 ml of trifluoroacetic acid at room temperature for 4 hours. The reaction solution is then neutralized with aqueous sodium bicarbonate solution, and the organic phase is separated off and dried over sodium sulfate. Filtration is followed by removal of the solvent in vacuo. 3.2 g (7.04 mmol, 92% yield) of a colorless oil are obtained which are employed in the next stage without further purification.

후처리

  1. customthe organic phase is separated off
  2. dry with materialdried over sodium sulfate
  3. filtrationFiltration
  4. customis followed by removal of the solvent in vacuo

출처 및 근거

ORD 기록
ord-ce317b1ed501428c99a18934d614935e
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998988B2

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