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

HRID 465660
ノート
印刷プレビュー

反応式

HRID 465660 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-8e5a20f04302476ab98ba1a8e823eb5a
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05153226

反応ノート

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