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

HRID 867078Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 867078
[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

Komponenten

4

Edukt 2

HCID 160352-Chloroethyl isocyanateHCID 83390(Dicyclopropylmethyl)amine

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-7e362a03602c4508823701aeddbc55a1
Quelldatensatz
uspto-grants-1978_07
Patentnummer
US04102890

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