2-Chloroethyl isocyanate → 1-(2-Chloroethyl)-3-(dicyclopropylmethyl)urea

HRID 867078ノート

反応式

HRID 867078 の反応式
[CH:1]1([CH:4]([NH2:8])[CH:5]2[CH2:7][CH2:6]2)[CH2:3][CH2:2]1.[Cl:9][CH2:10][CH2:11][N:12]=[C:13]=[O:14]>O1CCCC1>[CH:1]1([CH:4]([CH:5]2[CH2:7][CH2:6]2)[NH:8][C:13]([NH:12][CH2:11][CH2:10][Cl:9])=[O:14])[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 160352-Chloroethyl isocyanateHCID 83390(Dicyclopropylmethyl)amine

生成物 1

HCID 988261-(2-Chloroethyl)-3-(dicyclopropylmethyl)urea

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution made from 13.4 g of dicyclopropylmethylamine in 30 ml tetrahydrofuran is added dropwise to a solution of 13 g of β-chloroetyl isocyanate in 15 ml tetrahydrofuran while maintaining the inner temperature from 0° to +5° C. Then, the reaction mixture is kept at room temperature for 15 hours. Afterwards, the solution is evaporated to dryness and the dry residue, weighing 26.5 g, is used as such for the next step of the synthesis. For analytical purpose, a sample of the raw urea is recrystallised from acetonitrile. The N-(dicyclopropylmethyl) N-(β-chloroethyl) urea occurs as white crystals melting at 103°-104° C. with decomposition.

後処理

  1. temperaturewhile maintaining the inner temperature from 0° to +5° C
  2. customAfterwards, the solution is evaporated to dryness
  3. customsuch for the next step of the synthesis
  4. customFor analytical purpose, a sample of the raw urea is recrystallised from acetonitrile

出典と根拠

ORDレコード
ord-7e362a03602c4508823701aeddbc55a1
出典データセット
uspto-grants-1978_07
特許番号
US04102890

反応ノート

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