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Phosphorus sulfide (P2S5) → 3,4-dihydro-6-(3,4-dimethoxyphenyl)-1-ethyl-3-methyl-4-thioxo-2(1H)-pyrimidinone

HRID 621530
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HRID 621530 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[N:16]([CH2:17][CH3:18])[C:15](=[O:19])[N:14]([CH3:20])[C:13](=O)[CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:23]>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[N:16]([CH2:17][CH3:18])[C:15](=[O:19])[N:14]([CH3:20])[C:13](=[S:23])[CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
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참가 물질

4

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HCID 14817Phosphorus sulfide (P2S5)HCID 140964706-(3,4-dimethoxyphenyl)-1-ethyl-3-methyl-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 212432273,4-dihydro-6-(3,4-dimethoxyphenyl)-1-ethyl-3-methyl-4-thioxo-2(1H)-pyrimidinone수율 71.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 6-(3,4-dimethoxyphenyl)-1-ethyl-3-methyl-2,4(1H,3H)-pyrimidinedione (0.80 g) and phosphorus pentasulfide (1.8 g) in pyridine (18 ml) was refluxed for 15 hours with stirring. The reaction mixture was evaporated under reduced pressure. The residue was washed with 1N-hydrochloric acid and extracted with dichloromethane. The extract was washed with water, dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated in diisopropyl ether to give 3,4-dihydro-6-(3,4-dimethoxyphenyl)-1-ethyl-3-methyl-4-thioxo-2(1H)-pyrimidinone (0.60 g).

후처리

  1. temperaturewas refluxed for 15 hours
  2. customThe reaction mixture was evaporated under reduced pressure
  3. washThe residue was washed with 1N-hydrochloric acid
  4. extractionextracted with dichloromethane
  5. washThe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under reduced pressure
  8. customThe residue was triturated in diisopropyl ether

출처 및 근거

ORD 기록
ord-93264256817a4461826612849f27fcdb
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04824851

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