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

HRID 466944
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HRID 466944 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 280Carbon DioxideHCID 700EthanolamineHCID 8110Butyl isocyanate

생성물 1

HCID 2519951-Butyl-3-(2-hydroxyethyl)urea수율 113%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
30 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-e6adaa9225a7403292e04963affe31d5
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05158808

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