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

HRID 2380684

反応式

HRID 2380684 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-37e2e7bed79a4351a2f556e361619812
出典データセット
uspto-grants-1994_11
特許番号
US05369110

関連ノート

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