Ethanol → HCID 12791249, 화합물

HRID 1906154노트

반응식

HRID 1906154 반응식
[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[NH:6][CH:7]=1.Br[CH2:10][C:11]([C:13]1[S:14][C:15]([CH3:18])=[CH:16][CH:17]=1)=[O:12].C(O)C>C(N(CC)CC)C>[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[N:6]([CH2:10][C:11](=[O:12])[C:13]2[S:14][C:15]([CH3:18])=[CH:16][CH:17]=2)[CH:7]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 1085785-Chloro-2(1H)-pyrimidinoneHCID 122897372-Bromo-1-(5-methyl-2-thienyl)ethanone

생성물 1

HCID 12791249HCID 12791249, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

A mixture of 5-chloropyrimidin-2-one (522 mg) and 2-bromoacetyl-5-methylthiophene (1.30) g) in triethylamine (0.84 ml) and ethanol (25 ml) was stirred at room temperature. After 2 h. the mixture was concentrated to ca. 10 ml, diluted with ethyl acetate (100 ml), washed with water (×3) and brine, dried (MgSO4) and evaporated to a gum. The gum was triturated with diethyl ether and the resulting solid dissolved in ethanol and treated with charcoal. Evaporation of the solvent followed by recrystallisation of the residue twice from ethyl acetate gave the title pyrimidinone (205 mg) m.p. 199°-203° C., εmax (EtOH) 226.5 nm (ε8,570), 261.5 nm (ε9,280), 297 nm (ε11,630).

후처리

  1. concentrationAfter 2 h. the mixture was concentrated to ca. 10 ml
  2. additiondiluted with ethyl acetate (100 ml)
  3. washwashed with water (×3) and brine
  4. dry with materialdried (MgSO4)
  5. customevaporated to a gum
  6. customThe gum was triturated with diethyl ether
  7. dissolutionthe resulting solid dissolved in ethanol
  8. additiontreated with charcoal
  9. customEvaporation of the solvent
  10. customfollowed by recrystallisation of the residue twice from ethyl acetate

출처 및 근거

ORD 기록
ord-f05a06ceedf54610a75304f1a941df22
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04650800

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