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Water → 8-(2-chloroethylureido)-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran

HRID 2259882
ノート
印刷プレビュー

反応式

HRID 2259882 の反応式
[Cl:1][CH2:2][CH2:3][N:4]=[C:5]=[O:6].[NH2:7][C:8]1[C:17]2[O:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=2[CH:11]=[CH:10][CH:9]=1.O>CN(C)C=O>[Cl:1][CH2:2][CH2:3][NH:4][C:5](=[O:6])[NH:7][C:8]1[C:17]2[O:16][C:15]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=2[CH:11]=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 160352-Chloroethyl isocyanateHCID 199728088-amino-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran

生成物 1

HCID 677147128-(2-chloroethylureido)-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4 ml of 2-chloroethylisocyanate were added, under stirring at ambient temperature, to a solution of 3.9 g of 8-amino-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran in 52 ml of anhydrous dimethylformamide. Stirring was continued at 70° C. for 5 hours. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The organic phase was evaporated to dryness in vacuo. The residue was suspended in diethyl ether under stirring. The title product was then filtered off and recrystallized from methanol. Yield 3.74 g, m.p. 213°-214° C.

後処理

  1. extractionwas then extracted with ethyl acetate
  2. customThe organic phase was evaporated to dryness in vacuo
  3. stirringunder stirring
  4. filtrationThe title product was then filtered off
  5. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-00c74593a1a240c5abeea1aa5a5a5404
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05474994

反応ノート

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