反応 #595344

反応方程式

compound

2-(4-Chlorophenyl)-4,5-dimethyl-1,3-oxazole 3-oxide

phosphoryl chloride

ammonia

→

4-(Chloromethyl)-2-(4-chlorophenyl)-5-methyl-1,3-oxazole

溶媒

chloroform

反応条件

後処理

1. 1
   温度the reaction mixture is heated
2. 2
   温度at reflux for 30 min
3. 3
   抽出The mixture is extracted three times with in each case 20 ml of ethyl acetate
4. 4
   洗浄The combined organic phases are washed twice with in each case 5 ml of water
5. 5
   乾燥dried over magnesium sulfate
6. 6
   その他The solvent is removed on a rotary evaporator
7. 7
   その他The residue is used without further purification in the subsequent steps

実験手順

1.00 g (4.47 mmol) of the compound from Example 31A are initially charged in 15 ml of chloroform, and 1.5 ml (16.10 mmol) of phosphoryl chloride are added carefully. With stirring, the reaction mixture is heated at reflux for 30 min. The mixture is then cooled to 0° C. and made weakly basic by addition of ammonia. The mixture is extracted three times with in each case 20 ml of ethyl acetate. The combined organic phases are washed twice with in each case 5 ml of water and then dried over magnesium sulfate. The solvent is removed on a rotary evaporator. The residue is used without further purification in the subsequent steps.

出典