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

HRID 2258474ノート

反応式

HRID 2258474 の反応式
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

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178481542HCID 178481542、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-aef82a322e694f9892b773aefa64cf7c
出典データセット
uspto-grants-1997_08
特許番号
US05661153

反応ノート

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