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

HRID 2380676

반응식

HRID 2380676 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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)].

후처리

  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

출처 및 근거

ORD 기록
ord-7f19924fb62649ada6c2851fc4c9f959
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05369110

연결된 노트

불러오는 중…