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Propylamine → N-Butyl-N'-propylurea

HRID 466947
ノート
印刷プレビュー

反応式

HRID 466947 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7852PropylamineHCID 8110Butyl isocyanate

生成物 1

HCID 14836212N-Butyl-N'-propylurea収率 92.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-63ea547f32c14aacab029a3748b7bd11
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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