Phosphorus oxychloride → HCID 59312932、化合物

HRID 2389737ノート

反応式

HRID 2389737 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:14]=[C:13](O)[N:12]2[CH:16]=[CH:17][N:18]=[C:11]2[CH:10]=1.P(Cl)(Cl)([Cl:21])=O>C(=O)(O)[O-].[Na+]>[Cl:21][C:13]1[N:12]2[CH:16]=[CH:17][N:18]=[C:11]2[CH:10]=[C:9]([C:3]2[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=2[Cl:1])[N:14]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178517482HCID 178517482、化合物

生成物 1

HCID 59312932HCID 59312932、化合物

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒2 回

反応条件

温度
120 °C

実験手順

12.0 g (42.84 mmol) of 7-(2,4-dichlorophenyl)imidazo[1,2-c]pyrimidin-5-ol are introduced into 131.6 g (858.27 mmol) of phosphoryl chloride and heated at 120° C. for 5 h. A clear solution is produced after 10 min. The mixture is allowed to cool, and then 2000 ml of saturated aqueous sodium bicarbonate solution are cautiously added. Towards the end, about 100 g of solid sodium bicarbonate are also added, and the mixture is stirred at pH 7 for 10 min. The precipitate is filtered off with suction, thoroughly washed with water, suspended in a little isopropanol and sucked dry. It is then washed once more with petroleum ether and dried under high vacuum at 50° C. 11 g (81% of theory) of the product are obtained as a solid.

後処理

  1. customA clear solution is produced after 10 min
  2. temperatureto cool
  3. filtrationThe precipitate is filtered off with suction
  4. washthoroughly washed with water
  5. customsucked dry
  6. washIt is then washed once more with petroleum ether
  7. customdried under high vacuum at 50° C
  8. custom11 g (81% of theory) of the product are obtained as a solid

出典と根拠

ORDレコード
ord-18841ee676524ef0af30690db03f135b
出典データセット
uspto-grants-2012_09
特許番号
US08273752B2

反応ノート

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