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

HRID 1285151노트

반응식

HRID 1285151 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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].

후처리

  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

출처 및 근거

ORD 기록
ord-7a3c7f20eba045148278b3a13bd0ea97
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04565820

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