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

HRID 867078노트

반응식

HRID 867078 반응식
[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

참가 물질

4

반응물 2

HCID 160352-Chloroethyl isocyanateHCID 83390(Dicyclopropylmethyl)amine

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7e362a03602c4508823701aeddbc55a1
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04102890

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