Phosphorus oxychloride → 6-Chloro-3-methyl-1-phenylpyrimidine-2,4(1H,3H)-dione

HRID 2258474노트

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HRID 2258474 반응식
O[C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[CH:3]=1.P(Cl)(Cl)([Cl:19])=O>O>[Cl:19][C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[CH:3]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178481542HCID 178481542, 화합물

생성물 1

HCID 150462236-Chloro-3-methyl-1-phenylpyrimidine-2,4(1H,3H)-dione수율 72%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

To the obtained 6-hydroxy-3-methyl-1-phenyluracil (12.2 g, 56 mM) was added phosphorus oxychloride (phosphoryl chloride, 167 ml, 2M) under cooling with ice and 3.4 ml of water was then added dropwise. The solution was heated gradually and maintained at 110° C. for 2 hours. The solvent was distilled off under reduced pressure. A product was obtained by crystallization with water and recovered by filtration to yield 6-chloro-3-methyl-1-phenyluracil (yield: 9.55 g, or 72% based on 6-hydroxy-3-methyl-1-phenyluracil).

후처리

  1. additionwas then added dropwise
  2. temperatureThe solution was heated gradually
  3. distillationThe solvent was distilled off under reduced pressure
  4. customA product was obtained by crystallization with water
  5. filtrationrecovered by filtration

출처 및 근거

ORD 기록
ord-aef82a322e694f9892b773aefa64cf7c
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05661153

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