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

HRID 867079Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 867079
[CH:1]1([CH:4]([CH:12]2[CH2:14][CH2:13]2)[NH:5][C:6]([NH:8][CH2:9][CH2:10]Cl)=[O:7])[CH2:3][CH2:2]1>O>[CH:1]1([CH:4]([NH:5][C:6]2[O:7][CH2:10][CH2:9][N:8]=2)[CH:12]2[CH2:14][CH2:13]2)[CH2:3][CH2:2]1

Komponenten

3

Edukt 1

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

Produkt 1

HCID 68712Rilmenidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

25 g of raw urea obtained by step (a) are suspended in 150 ml of water and heated under reflux for 2 hours. After allowing the temperature of the mixture to return to room temperature, the aqueous solution is extracted with ether. The aqueous phase is separated and made alkaline by adding concentrated ammonia. The resulting precipitate is separated by suction, washed with water and dried. 11.8 g of 2-(dicyclopropylmethylamino) oxazoline are thus recovered, melting at 105°-106° C. A mixture of the latter with N-(dicyclopropylmethyl) N'-(β-chloroethyl) urea gives a decrease of the melting point.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 2 hours
  3. customto return to room temperature
  4. extractionthe aqueous solution is extracted with ether
  5. customThe aqueous phase is separated
  6. additionby adding concentrated ammonia
  7. customThe resulting precipitate is separated by suction
  8. washwashed with water
  9. customdried
  10. custom11.8 g of 2-(dicyclopropylmethylamino) oxazoline are thus recovered
  11. additionA mixture of the latter with N-(dicyclopropylmethyl) N'-(β-chloroethyl) urea
  12. customgives a decrease of the melting point

Quellen und Nachweise

ORD-Eintrag
ord-dc15fe349c0b4c3993036749d88684bd
Quelldatensatz
uspto-grants-1978_07
Patentnummer
US04102890

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