Hydrogen Bromide → 5-Ethyl-5-(3-bromopropyl)barbituric acid

HRID 1195204ノート

反応式

HRID 1195204 の反応式
[CH2:1]([C:3]1([CH2:12][CH:13]=[CH2:14])[C:8](=[O:9])[NH:7][C:6](=[O:10])[NH:5][C:4]1=[O:11])[CH3:2].[BrH:15]>C1(C)C=CC=CC=1>[CH2:1]([C:3]1([CH2:12][CH2:13][CH2:14][Br:15])[C:4](=[O:11])[NH:5][C:6](=[O:10])[NH:7][C:8]1=[O:9])[CH3:2]

参加物

4

反応物 2

HCID 260Hydrogen Bromide2 回HCID 485422,4,6(1H,3H,5H)-Pyrimidinetrione, 5-ethyl-5-(2-propenyl)-

生成物 1

HCID 199118015-Ethyl-5-(3-bromopropyl)barbituric acid

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A suspension of 40 g of 5-ethyl-5-allylbarbituric acid and 800 ml of toluene was stirred and irradiated with a GE sunlamp (275 watts, 110-125 volts) for approximately 90 min. Thereafter, gaseous HBr was passed for 45 min. with further irradiation and stirred for another 45 minutes. The reaction flask was then opened to allow the excess HBr to evaporate. The solution was cooled and filtered. The resulting precipitate was washed with toluene, dried, and then dissolved in a minimal amount of hot acetone. Petroleum ether (60°-68° C.) was added until a small amount of precipitate appeared; the flask was left overnight at 23° C. The crystals were filtered, washed with petroleum ether, and air dried. The melting point was 138°-140° C.

後処理

  1. customirradiated with a GE sunlamp (275 watts, 110-125 volts) for approximately 90 min
  2. stirringstirred for another 45 minutes
  3. customto evaporate
  4. temperatureThe solution was cooled
  5. filtrationfiltered
  6. washThe resulting precipitate was washed with toluene
  7. customdried
  8. dissolutiondissolved in a minimal amount of hot acetone
  9. additionPetroleum ether (60°-68° C.) was added until a small amount of precipitate
  10. filtrationThe crystals were filtered
  11. washwashed with petroleum ether, and air
  12. customdried

出典と根拠

ORDレコード
ord-88bd73ad002446f4ae22af412c49a706
出典データセット
uspto-grants-1992_05
特許番号
US05110914

反応ノート

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