تفاعل #595343

ord-206771c8f13e40dd8874837b02bbecb1

معادلة التفاعل

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

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture is heated
  2. 2
    درجة الحرارةto reflux
  3. 3
    استخلاصThe reaction mixture is extracted three times with in each case 20 ml of ethyl acetate
  4. 4
    أخرىThe solvent is removed on a rotary evaporator
  5. 5
    أخرىthe residue is dried in a vacuum
  6. 6
    أخرىdrying cabinet
  7. 7
    أخرىThe product is used without further purification in the subsequent reactions

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09095582B2uspto-grants-2015_08