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2-Methoxybenzoyl chloride → N-[2-[[2,6-bis(1-Methylethyl)phenyl]amino]-2-oxoethyl]-N-(diphenylmethyl)-2-methoxybenzamide

HRID 465660
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HRID 465660 반응식
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[C:5](Cl)=[O:6].[CH3:12][CH:13]([C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([CH:21]([CH3:23])[CH3:22])[C:16]=1[NH:24][C:25](=[O:41])[CH2:26][NH:27][CH:28]([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[CH3:14]>C(N(CC)CC)C>[CH3:14][CH:13]([C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([CH:21]([CH3:22])[CH3:23])[C:16]=1[NH:24][C:25](=[O:41])[CH2:26][N:27]([CH:28]([C:35]1[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1)[C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[C:5](=[O:6])[C:4]1[CH:8]=[CH:9][CH:10]=[CH:11][C:3]=1[O:2][CH3:1])[CH3:12]
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참가 물질

4

반응물 2

HCID 889692-Methoxybenzoyl chlorideHCID 1645639N-[2,6-bis(1-Methylethyl)phenyl]-2-[(diphenylmethyl)amino]acetamide

생성물 1

HCID 19874995N-[2-[[2,6-bis(1-Methylethyl)phenyl]amino]-2-oxoethyl]-N-(diphenylmethyl)-2-methoxybenzamide

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

2-Methoxy benzoyl chloride (0.65 g) was added to a mixture of 1.50 g the product of Example 4 and excess triethylamine in 100 mL EtoAc. The reaction mixture was allowed to sit 2 days at room temperature and was then concentrated to dryness, the residue dissolved in 250 mL CH2Cl2, the organic solution washed with dilute sulfuric acid, brine, potassium carbonate solution, and brine. The solution was dried over MgSO4, filtered, and concentrated to an oil which crystallized upon addition of 1/1, hexane/EtoAc to give the title compound. Total yield, 1.53 g (76%).

후처리

  1. concentrationwas then concentrated to dryness
  2. dissolutionthe residue dissolved in 250 mL CH2Cl2
  3. washthe organic solution washed with dilute sulfuric acid, brine, potassium carbonate solution, and brine
  4. dry with materialThe solution was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated to an oil which
  7. customcrystallized upon addition of 1/1, hexane/EtoAc

출처 및 근거

ORD 기록
ord-8e5a20f04302476ab98ba1a8e823eb5a
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05153226

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