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

HRID 867079ノート

反応式

HRID 867079 の反応式
[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

参加物

3

反応物 1

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

生成物 1

HCID 68712Rilmenidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dc15fe349c0b4c3993036749d88684bd
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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