Triethylamine → 3,3-dimethyl-4-methoxycarbonyl-butanoic acid N-(2'-cyanobiphenyl-4-ylmethyl)-N-propyl-amide

HRID 2380676ノート

反応式

HRID 2380676 の反応式
C(N(CC)CC)C.[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[CH:21]=[CH:20][C:19]([CH2:22][NH:23][CH2:24][CH2:25][CH3:26])=[CH:18][CH:17]=1)#[N:9].[Cl-].[CH3:28][O:29][C:30](=[O:39])[CH2:31][C:32]([CH3:38])([CH3:37])[CH2:33][C:34]([OH:36])=O>C(Cl)Cl>[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[CH:17]=[CH:18][C:19]([CH2:22][N:23]([CH2:24][CH2:25][CH3:26])[C:34](=[O:36])[CH2:33][C:32]([CH3:38])([CH3:37])[CH2:31][C:30]([O:29][CH3:28])=[O:39])=[CH:20][CH:21]=1)#[N:9]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 15338355N-(2'-cyanobiphenyl-4-ylmethyl)-N-propyl-amineHCID 867482873,3-Dimethylglutaric acid monomethyl ester monochloride

生成物 1

HCID 536371373,3-dimethyl-4-methoxycarbonyl-butanoic acid N-(2'-cyanobiphenyl-4-ylmethyl)-N-propyl-amide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.83 ml of triethylamine are added to a solution of 2.19 g of N-(2'-cyanobiphenyl-4-ylmethyl)-N-propyl-amine and 2.37 g of 3,3-dimethylglutaric acid monomethyl ester monochloride in 100 ml of CH2Cl2 and the mixture is stirred at room temperature for 2 hours. Extraction twice with 50 ml of water each time and extraction of the aqueous phase with 40 ml of CH2Cl2 produces an organic phase which, after being concentrated by evaporation, yields by the customary procedure 3,3-dimethyl-4-methoxycarbonyl-butanoic acid N-(2'-cyanobiphenyl-4-ylmethyl)-N-propyl-amide that has an Rf value of 0.66 [CH2Cl2 /CH3OH (95:5)].

後処理

  1. extractionExtraction twice with 50 ml of water
  2. extractioneach time and extraction of the aqueous phase with 40 ml of CH2Cl2
  3. customproduces an organic phase which
  4. concentrationafter being concentrated by evaporation

出典と根拠

ORDレコード
ord-7f19924fb62649ada6c2851fc4c9f959
出典データセット
uspto-grants-1994_11
特許番号
US05369110

反応ノート

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