Acetic Acid → 2-[2-(4-Benzyloxyphenyl)ethyl]amino-alpha-(3-tert-butoxycarbonylaminomethylphenyl)-5-chloro-benzyl alcohol

HRID 275866

반응식

HRID 275866 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH:16]=O)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)(=O)C.[H-].C([Na])#N.[NH2:26][C:27]1[CH:49]=[CH:48][C:47]([Cl:50])=[CH:46][C:28]=1[CH:29]([OH:45])[C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([CH2:36][NH:37][C:38]([O:40][C:41]([CH3:44])([CH3:43])[CH3:42])=[O:39])[CH:31]=1>CO.C(OCC)(=O)C>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:15][CH2:16][NH:26][C:27]2[CH:49]=[CH:48][C:47]([Cl:50])=[CH:46][C:28]=2[CH:29]([OH:45])[C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([CH2:36][NH:37][C:38]([O:40][C:41]([CH3:43])([CH3:44])[CH3:42])=[O:39])[CH:31]=2)=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

7

반응 조건

온도
60 °C

실험 절차

In methanol (15 ml) were dissolved 2-amino-5-chloro-α-(3-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol produced in Example 1-(2) (0.5 g) and 4-benzyloxyphenylacetaldehyde (0.4 g). To the solution were added acetic acid (0.1 g) and, subsequently, cyano sodium hydride (0.11 g). The mixture was stirred for 40 minutes at 60° C. The reaction mixture was diluted with ethyl acetate (60 ml), which was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off to leave 2-[2-(4-benzyloxyphenyl)ethyl]amino-α-(3-tert-butoxycarbonylaminomethylphenyl)-5-chloro-benzyl alcohol (0.45 g) as a colorless oily product.

후처리

  1. washwas washed with water
  2. dry with materialdried over anhydrous sodium sulfate
  3. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-1c8c5b7df28743a49d051f48e5d4a748
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06352982B1

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