Urea → HCID 178517841、化合物

HRID 1831050

反応式

HRID 1831050 の反応式
[O-]CC.[Na+].[Na].[Cl:6][C:7]1[CH:8]=[C:9]([CH:18]=[CH:19][C:20]=1[Cl:21])[O:10][C:11](=[CH:14]N(C)C)[CH:12]=O.[NH2:22][C:23]([NH2:25])=[O:24]>C(O)C.C(O)(=O)C.O>[Cl:6][C:7]1[CH:8]=[C:9]([CH:18]=[CH:19][C:20]=1[Cl:21])[O:10][C:11]1[CH:14]=[N:22][C:23]([OH:24])=[N:25][CH:12]=1

参加物

8

反応物 4

HCID 1176UreaHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 545558182-(3,4-Dichlorophenoxy)-3-(dimethylamino)prop-2-enal

生成物 1

HCID 178517841HCID 178517841、化合物収率 17.3%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

A solution of sodium ethoxide, prepared from sodium (0.95 g, 41.4 mmol), 2-(3,4-dichloro-phenoxy)-3-dimethylamino-propenal (5.38 g, 20.7 mmol) and urea (2.48 g, 41.4 mmol) in ethanol (25 ml) was heated at 60° C. for 4 hours. Water (1 ml) was added and heating was continued for an additional 2 hours. The solution was cooled to room temperature and neutralised with glacial acetic acid. Most of the solvent was removed by evaporation in vacuo. Water was added and the precipitate was isolated by suction, followed by drying in a vacuum oven, yielding the title compound (0.92 g, 17% yield) as a brown solid.

後処理

  1. temperatureheating
  2. customMost of the solvent was removed by evaporation in vacuo
  3. additionWater was added
  4. customthe precipitate was isolated by suction
  5. customby drying in a vacuum oven

出典と根拠

ORDレコード
ord-833b3decc98144cca4e5174dcc2a9b6b
出典データセット
uspto-grants-2006_06
特許番号
US07067517B2

関連ノート

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