反応 #595343

ord-206771c8f13e40dd8874837b02bbecb1

反応方程式

CCc1oc(-c2ccc(Cl)cc2)[n+]([O-])c1C
compound
CCc1oc(-c2ccc(Cl)cc2)[n+]([O-])c1C
2-(4-Chlorophenyl)-5-ethyl-4-methyl-1,3-oxazole 3-oxide
O=P(Cl)(Cl)Cl
phosphoryl chloride
N
ammonia
CCc1oc(-c2ccc(Cl)cc2)nc1CCl
4-(Chloromethyl)-2-(4-chlorophenyl)-5-ethyl-1,3-oxazole

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture is heated
  2. 2
    温度to reflux
  3. 3
    抽出The reaction mixture is extracted three times with in each case 20 ml of ethyl acetate
  4. 4
    その他The solvent is removed on a rotary evaporator
  5. 5
    その他the residue is dried in a vacuum
  6. 6
    その他drying cabinet
  7. 7
    その他The product is used without further purification in the subsequent reactions

実験手順

1.00 g (4.21 mmol) of the compound from Example 29A are dissolved in 15 ml of chloroform, and 1.4 ml (15.15 mmol) of phosphoryl chloride are added carefully. The mixture is heated to reflux and stirred at this temperature for 30 min. The mixture is then cooled to 0° C. and made slightly basic using ammonia. The reaction mixture is extracted three times with in each case 20 ml of ethyl acetate. The solvent is removed on a rotary evaporator and the residue is dried in a vacuum drying cabinet. The product is used without further purification in the subsequent reactions.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09095582B2uspto-grants-2015_08