Hydrochloric Acid → Ethyl 2-chloro-5-{3-[2-(ethoxycarbonyl)vinyl]ureido}-benzoate

HRID 1252969

反応式

HRID 1252969 の反応式
[Cl:1][C:2]1[CH:12]=[CH:11][C:10]([NH:13][C:14]([NH2:16])=[O:15])=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].C(O[CH:20]=[CH:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])C.Cl>COCCOC>[Cl:1][C:2]1[CH:12]=[CH:11][C:10]([NH:13][C:14]([NH:16][CH:20]=[CH:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])=[O:15])=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5]

参加物

5

実験手順

6.0 g of ethyl 2-chloro-5-ureidobenzoate and 6.4 g of ethyl 3-ethoxyacrylate are heated at reflux temperature in 100 ml of 1,2-dimethoxyethane and subsequently heated at this temperature with 12 ml of 2N hydrochloric acid for 5 minutes. The reaction mixture is evaporated to dryness under reduced pressure and the residue is purified by chromatography on 300 g of silica gel using ethyl acetate/n-hexane (1:3) as the eluent. There is obtained ethyl 2-chloro-5-{3-[2-(ethoxycarbonyl)vinyl]ureido}-benzoate, m.p. 116°-117° C.

後処理

  1. customThe reaction mixture is evaporated to dryness under reduced pressure
  2. customthe residue is purified by chromatography on 300 g of silica gel

出典と根拠

ORDレコード
ord-44d22b3f272f45bc8bd880d0d851fd2a
出典データセット
uspto-grants-1988_05
特許番号
US04746352

関連ノート

読み込み中…