반응 #595344

반응 방정식

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

용매

chloroform

반응 조건

후처리

1. 1
   온도the reaction mixture is heated
2. 2
   온도at reflux for 30 min
3. 3
   추출The mixture is extracted three times with in each case 20 ml of ethyl acetate
4. 4
   세척The combined organic phases are washed twice with in each case 5 ml of water
5. 5
   건조dried over magnesium sulfate
6. 6
   기타The solvent is removed on a rotary evaporator
7. 7
   기타The residue is used without further purification in the subsequent steps

실험 절차

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.

출처