Homophthalic anhydride → 2-carboxy-phenylacetic acid N-butyl-N-(2'-cyanobiphenyl-4-ylmethyl)-amide

HRID 2380684

반응식

HRID 2380684 반응식
[CH2:1]([NH:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[C:19]#[N:20])=[CH:9][CH:8]=1)[CH2:2][CH2:3][CH3:4].[C:21]1(=[O:32])[O:27][C:25](=[O:26])[C:24]2=[CH:28][CH:29]=[CH:30][CH:31]=[C:23]2[CH2:22]1.C(Cl)Cl.CCOCC.CCCCCC>O1CCOCC1>[CH2:1]([N:5]([CH2:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[C:19]#[N:20])=[CH:9][CH:8]=1)[C:21](=[O:32])[CH2:22][C:23]1[CH:31]=[CH:30][CH:29]=[CH:28][C:24]=1[C:25]([OH:27])=[O:26])[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 3

HCID 12801Homophthalic anhydrideHCID 153383534'-Butylaminomethyl-2-cyanobiphenylHCID 21850893Dichloromethane ether hexane

생성물 1

HCID 539424252-carboxy-phenylacetic acid N-butyl-N-(2'-cyanobiphenyl-4-ylmethyl)-amide

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

The starting material can be prepared, for example, as follows: A solution of 2.64 g of N-butyl-N-(2'-cyanobiphenyl-4-ylmethyl)-amine and 2.43 g of homophthalic acid anhydride in 50 ml of dioxane is heated under reflux for hour. After removal of the solvent, the residue is taken up in 100 ml of ethyl acetate and washed twice with 50 ml of water each time. After customary treatment, the organic phase yields a crude product that yields, from CH2Cl2 /ether/hexane, 2-carboxy-phenylacetic acid N-butyl-N-(2'-cyanobiphenyl-4-ylmethyl)-amide, m.p. 137°-139°.

후처리

  1. temperatureunder reflux for hour
  2. customAfter removal of the solvent
  3. washwashed twice with 50 ml of water each time
  4. customAfter customary treatment, the organic phase yields a crude product

출처 및 근거

ORD 기록
ord-37e2e7bed79a4351a2f556e361619812
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05369110

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