Sodium Hydroxide → 4-Chloro-6-methyl-2-(propan-2-yl)pyrimidine

HRID 14345

反応式

HRID 14345 の反応式
[CH:1]([C:4]1[N:9]=[C:8](O)[CH:7]=[C:6]([CH3:11])[N:5]=1)([CH3:3])[CH3:2].P(Cl)(Cl)([Cl:14])=O.[OH-].[Na+]>C1(C)C=CC=CC=1>[Cl:14][C:8]1[CH:7]=[C:6]([CH3:11])[N:5]=[C:4]([CH:1]([CH3:3])[CH3:2])[N:9]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 178419104HCID 178419104、化合物

生成物 1

HCID 33069074-Chloro-6-methyl-2-(propan-2-yl)pyrimidine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

76.1 g of 2-isopropyl-6-methyl-4-pyrimidinol [2814-20-2] (500 mmol) are dissolved in 300 ml of toluene at 90° C. 80.5 g of phosphorus oxychloride (525 mmol) are added dropwise thereto at from 90 to 103° C., and the reaction mixture is heated at 110° C. for 2 hours. After cooling to 20° C., the reaction mixture is adjusted to pH 8 using 4M sodium hydroxide solution, with cooling. The aqueous phase is separated off and extracted with 100 ml of toluene. The combined organic phases are washed three times with 100 ml of water each time and dried at RT under 2 mbar. 89.7 g (105%; contains toluene) are obtained.

後処理

  1. temperatureAfter cooling to 20° C.
  2. temperaturewith cooling
  3. customThe aqueous phase is separated off
  4. extractionextracted with 100 ml of toluene
  5. washThe combined organic phases are washed three times with 100 ml of water each time
  6. customdried at RT under 2 mbar
  7. custom89.7 g (105%; contains toluene) are obtained

出典と根拠

ORDレコード
ord-c1733baf1fbe4d7cba07485c4f3375fa
出典データセット
uspto-grants-2010_06
特許番号
US07731985B2

関連ノート

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