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Propylamine → N-Butyl-N'-propylurea

HRID 466947
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HRID 466947 반응식
[CH2:1]([NH2:4])[CH2:2][CH3:3].[CH2:5]([N:9]=[C:10]=[O:11])[CH2:6][CH2:7][CH3:8]>ClCCl>[CH2:1]([NH:4][C:10]([NH:9][CH2:5][CH2:6][CH2:7][CH3:8])=[O:11])[CH2:2][CH3:3]
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참가 물질

4

반응물 2

HCID 7852PropylamineHCID 8110Butyl isocyanate

생성물 1

HCID 14836212N-Butyl-N'-propylurea수율 92.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

205.8 Grams (3.48 moles) of n-propylamine and 250 ml of dichloromethane were charged to a round bottom flask equipped with stirrer, thermometer, reflux condenser and dropping funnel. 313.7 Grams (3.16 moles) of butyl isocyanate were added to the dropping funnel and then metered into the flask with stirring and strong external cooling (solid CO2 bath) at a rate slow enough to maintain the contents generally below 0° C. except for brief excursions to higher temperatures. The resulting mixture was left to stand overnight and then freed of solvent and lights under vacuum with a rotary evaporator leaving 462.3 g of crude product (92.6% crude yield). After further drying of a portion under vacuum a 97.6 area % purity was recorded by gas chromatography. The product contained substantially only one compound by gas chromatography. It melted at 70°-72° C.

후처리

  1. customequipped with stirrer
  2. temperaturethermometer, reflux condenser
  3. temperaturestrong external cooling (solid CO2 bath) at a rate slow enough
  4. temperatureto maintain the contents generally below 0° C. except for brief excursions to higher temperatures
  5. waitThe resulting mixture was left
  6. customfreed of solvent and lights under vacuum with a rotary evaporator

출처 및 근거

ORD 기록
ord-63ea547f32c14aacab029a3748b7bd11
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05158808

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