Sodium Hydroxide → 7-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

HRID 72376

反応式

HRID 72376 の反応式
O[C:2]1[N:3]=[C:4]2[NH:11][C:10]([CH3:13])([CH3:12])[CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1.P(Cl)(Cl)([Cl:16])=O.[OH-].[Na+]>>[Cl:16][C:2]1[N:3]=[C:4]2[NH:11][C:10]([CH3:13])([CH3:12])[CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1

参加物

4

反応物 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 136269314HCID 136269314、化合物

生成物 1

HCID 1363591007-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

反応条件

温度
120 °C

実験手順

4.5 g of 7-hydroxy-2,2-dimethyl-2,3-dihydro-1H-imidazo[1,2-a]pyrimidin-5-one and 35 ml of phosphorus oxychloride are introduced into a round-bottomed flask. The resulting mixture is then heated at 120° C. for three hours. After cooling, the reaction mixture is concentrated to dryness under reduced pressure. Ice is added to the residue obtained, and then concentrated sodium hydroxide is added until a pH in the region of 5-6 is obtained. The solid formed is filtered off so as to give 1 g of 7-chloro-2,2-dimethyl-2,3-dihydro-1H-imidazo[1,2-a]pyrimidin-5-one, in the form of a brown solid, the characteristics of which are the following:

後処理

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture is concentrated to dryness under reduced pressure
  3. additionIce is added to the residue
  4. customobtained
  5. customis obtained
  6. customThe solid formed
  7. filtrationis filtered off so as

出典と根拠

ORDレコード
ord-ed9beb56a5f14bc88be5c87a157d8a9b
出典データセット
uspto-grants-2014_09
特許番号
US08828997B2

関連ノート

読み込み中…