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Ethanolamine → 1-Butyl-3-(2-hydroxyethyl)urea

HRID 1194462
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HRID 1194462 반응식
[CH2:1]([CH2:3][NH2:4])[OH:2].[CH2:5]([N:9]=[C:10]=[O:11])[CH2:6][CH2:7][CH3:8]>ClCCl>[OH:2][CH2:1][CH2:3][NH:4][C:10]([NH:9][CH2:5][CH2:6][CH2:7][CH3:8])=[O:11]
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참가 물질

4

반응물 2

HCID 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 at 99% purity) of ethanolamine and 170 grams of dichloromethane were charged to a flask eguipped with stirrer, thermometer, feed tank, distillation head and condenser. 101 grams (1 mole at 98% purity) of butyl isocyanate were fed to the flask dropwise with stirring and cooling (utilizing a dry ice bath) over a period of 1.5 hours 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 flask contents were 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 was recrystallized from 2-butanone giving tiny white crystals melting at 67° C. The HLB value of N-(2-hydroxyethyl)-N'-1-butyl urea is 12.9.

후처리

  1. customeguipped with stirrer
  2. distillationthermometer, feed tank, distillation head and condenser
  3. temperaturecooling (utilizing a dry ice bath) over a period of 1.5 hours such that the temperature of the reaction mixture
  4. customAt this time some solid had been formed
  5. dissolutionit was redissolved
  6. temperatureby heating to 46° C
  7. stirringThe flask contents were stirred at 46° C. for an additional two hours
  8. customby stripping at 90° C.

출처 및 근거

ORD 기록
ord-0c5244f1ffe9441cb3bc450bf554dffa
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04814382

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