Hydrochloric Acid → Barbituric Acid

HRID 580551

反応式

HRID 580551 の反応式
N1C=CC=C1.[K].ICCCC.[NH:12]1[C:20](=[O:21])[C:18](=O)[C:16](=[O:17])[NH:15][C:13]1=[O:14].Cl>C(O)C.O1CCCC1>[NH:12]1[C:20](=[O:21])[CH2:18][C:16](=[O:17])[NH:15][C:13]1=[O:14]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 5781AlloxanHCID 10962Butyl iodideHCID 241923201H-Pyrrole, potassium salt (1:1)

生成物 1

HCID 6211Barbituric Acid収率 132.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Potassium pyrrole (3.0 g., 0.03 mole), 1-iodobutane (9.2 g., 0.05 moles) and 10 ml. of tetrahydrofuran were combined and refluxed for 1.5 hours by which time the reaction mixture had become a thick mass. The reaction mixture was diluted with 30 ml. of water and extracted with 35 ml. of ether. The ether was backwashed with water, then added to a solution of anhydrous alloxan (4.8 g., 0.03 mole) obtained by heating in 50 ml. of ethanol. The ether was distilled away, 6N hydrochloric acid (5 ml., 0.03 mole) was added, and the mixture refluxed for 3 minutes, cooled, evaporated to a gum, and triturated with water to afford title product [5.1 g.; m.p. 135 (dec); m/e 265].

後処理

  1. temperaturerefluxed for 1.5 hours by which time the reaction mixture
  2. additionThe reaction mixture was diluted with 30 ml
  3. extractionof water and extracted with 35 ml
  4. customobtained
  5. temperatureby heating in 50 ml
  6. distillationThe ether was distilled away
  7. temperaturethe mixture refluxed for 3 minutes
  8. temperaturecooled
  9. customevaporated to a gum
  10. customtriturated with water

出典と根拠

ORDレコード
ord-fd3679523c564aca9f8f87d8fbc6713d
出典データセット
uspto-grants-1988_06
特許番号
US04753956

関連ノート

読み込み中…