Ethanol → HCID 12791249、化合物

HRID 1906154ノート

反応式

HRID 1906154 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 12791249HCID 12791249、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f05a06ceedf54610a75304f1a941df22
出典データセット
uspto-grants-1987_03
特許番号
US04650800

反応ノート

読み込み中…