Hydrochloric Acid → 5-Hydroxy-5-[1-(1-butyl)-2-pyrrolyl)-2,4,6-(1H,3H,5H)pyrimidinetrione

HRID 66591

反応式

HRID 66591 の反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[K].I[CH2:8][CH2:9][CH2:10][CH3:11].[NH:12]1[C:20](=[O:21])[C:18](=[O:19])[C:16](=[O:17])[NH:15][C:13]1=[O:14].Cl>C(O)C.O1CCCC1>[OH:19][C:18]1([C:2]2[N:1]([CH2:8][CH2:9][CH2:10][CH3:11])[CH:5]=[CH:4][CH:3]=2)[C:16](=[O:17])[NH:15][C:13](=[O:14])[NH:12][C:20]1=[O:21]

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 132828935-Hydroxy-5-[1-(1-butyl)-2-pyrrolyl)-2,4,6-(1H,3H,5H)pyrimidinetrione収率 64.1%

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 back-washed 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, 6 N 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. washThe ether was back-washed with water
  5. customobtained
  6. temperatureby heating in 50 ml
  7. distillationThe ether was distilled away
  8. temperaturethe mixture refluxed for 3 minutes
  9. temperaturecooled
  10. customevaporated to a gum
  11. customtriturated with water

出典と根拠

ORDレコード
ord-9d9bd77c87eb40fe84919dff7e53f81f
出典データセット
uspto-grants-1982_08
特許番号
US04342771

関連ノート

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