تفاعل #595344

ord-867345793a3c4a99be0f169b1582f752

معادلة التفاعل

Cc1oc(-c2ccc(Cl)cc2)[n+]([O-])c1C
compound
Cc1oc(-c2ccc(Cl)cc2)[n+]([O-])c1C
2-(4-Chlorophenyl)-4,5-dimethyl-1,3-oxazole 3-oxide
O=P(Cl)(Cl)Cl
phosphoryl chloride
N
ammonia
Cc1oc(-c2ccc(Cl)cc2)nc1CCl
4-(Chloromethyl)-2-(4-chlorophenyl)-5-methyl-1,3-oxazole

المذيبات

ظروف التفاعل

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

المعالجة

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

الإجراء التجريبي

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.

المصدر

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