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Carbon Dioxide → 1-Butyl-3-(2-hydroxyethyl)urea

HRID 466944
ノート
印刷プレビュー

反応式

HRID 466944 の反応式
[CH2:1]([CH2:3][NH2:4])[OH:2].[CH2:5]([N:9]=[C:10]=[O:11])[CH2:6][CH2:7][CH3:8].C(=O)=O>ClCCl>[OH:2][CH2:1][CH2:3][NH:4][C:10]([NH:9][CH2:5][CH2:6][CH2:7][CH3:8])=[O:11]
参加物反応条件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 280Carbon DioxideHCID 700EthanolamineHCID 8110Butyl isocyanate

生成物 1

HCID 2519951-Butyl-3-(2-hydroxyethyl)urea収率 113%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
30 °C

実験手順

61.7 Grams (1 mole @ 99% purity) of ethanolamine and 170 grams of dichloromethane were charged to a flask equipped with stirrer, thermometer, feed tank, distillation head and condenser. 101 Grams (1 mole @ 98% purity) of butyl isocynate were fed dropwise with stirring and cooling (dry ice bath) during 1.5 hrs. such that the temperature of the reaction mixture was maintained at about 30° C. At this time some solid had been formed and it was redissolved by heating to 46° C. The mixture was stirred at 46° C. for an additional two hours and then freed of volatile materials by stripping at 90° C. and 2 mm Hg leaving 181 g of solid product. This material could be recrystallized from 2-butanone giving tiny white crystals melting at 67° C.

後処理

  1. customequipped with stirrer
  2. distillationthermometer, feed tank, distillation head and condenser
  3. customAt this time some solid had been formed
  4. dissolutionit was redissolved
  5. temperatureby heating to 46° C
  6. stirringThe mixture was stirred at 46° C. for an additional two hours
  7. customby stripping at 90° C.

出典と根拠

ORDレコード
ord-e6adaa9225a7403292e04963affe31d5
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05158808

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート