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

HRID 980188

반응식

HRID 980188 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 127955605-Chloro-1-desylpyrimidin-2-one수율 40.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8471Triethylamine용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-2905d1c3fd6d472aaa0b555daf5e4aae
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04636509

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