반응 #595343

ord-206771c8f13e40dd8874837b02bbecb1

반응 방정식

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

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture is heated
  2. 2
    온도to reflux
  3. 3
    추출The reaction mixture is extracted three times with in each case 20 ml of ethyl acetate
  4. 4
    기타The solvent is removed on a rotary evaporator
  5. 5
    기타the residue is dried in a vacuum
  6. 6
    기타drying cabinet
  7. 7
    기타The product is used without further purification in the subsequent reactions

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09095582B2uspto-grants-2015_08