Ethanone, 2-chloro-1,2-diphenyl- → 5-Chloro-1-desylpyrimidin-2-one

HRID 980188

反応式

HRID 980188 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[NH:6][CH:7]=1.[C:9]1([C:15]([CH:17](Cl)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[O:16])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>C(N(CC)CC)C.C(O)C>[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[N:6]([CH:17]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:15](=[O:16])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=1

参加物

5

反応物 2

HCID 95343Ethanone, 2-chloro-1,2-diphenyl-HCID 1085785-Chloro-2(1H)-pyrimidinone

生成物 1

HCID 127955605-Chloro-1-desylpyrimidin-2-one収率 40.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8471Triethylamine溶媒

実験手順

A solution of 5-chloropyrimidin-2-one (406 mg) and desyl chloride (2-chloro-2-phenyl acetophenone) (692 mg) in triethylamine (1 ml) and ethanol (20 ml) was stirred at ambient temperature for one hour, then heated at reflux for 11/2 hours. After evaporation of solvents, the residue was dissolved in ethyl acetate (150 ml). The solution was washed with water (100 ml), dried (MgSO4) and evaporated to a foam which was crystallised from ethyl acetate to give the title pyrimidinone (393 mg,); m.p. 145°-146°; λmaxEtOH 230 nm (ε 15960), 250 nm (ε 15000), 335 nm (ε 4700), λinf 262.5 nm (ε 8400), 269 n, (ε 4420).

後処理

  1. temperatureheated
  2. temperatureat reflux for 11/2 hours
  3. customAfter evaporation of solvents
  4. dissolutionthe residue was dissolved in ethyl acetate (150 ml)
  5. washThe solution was washed with water (100 ml)
  6. dry with materialdried (MgSO4)
  7. customevaporated to a foam which
  8. customwas crystallised from ethyl acetate

出典と根拠

ORDレコード
ord-2905d1c3fd6d472aaa0b555daf5e4aae
出典データセット
uspto-grants-1987_01
特許番号
US04636509

関連ノート

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