Methane → 4-(Cyanomethoxy)benzonitrile

HRID 66765

반응식

HRID 66765 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1)#[N:2].C([O-])([O-])=O.[K+].[K+].Cl[CH2:17][C:18]#[N:19].C>CC(Cl)(Cl)Cl.O.CN(C)C=O>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([O:9][CH2:17][C:18]#[N:19])=[CH:5][CH:4]=1)#[N:2]

참가 물질

8

반응물 4

HCID 297MethaneHCID 7856ChloroacetonitrileHCID 11430Potassium CarbonateHCID 130194-Cyanophenol

생성물 1

HCID 205290614-(Cyanomethoxy)benzonitrile

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 62781,1,1-Trichloroethane용매

반응 조건

온도
5 °C

실험 절차

The compound of 4-cyanophenoxyacetonitrile was prepared by heating 29.8 g of 4-cyanophenol, 44.8 g of anhydrous K2CO3, 40 ml of dimethylformamide and 18.75 g of chloroacetonitrile with stirring in a round-bottomed three-necked flask at 70°-80° C. for 3 hours, after which time the reaction mixture was poured into an ice and water mixture, which resulted in crystal formation. The crystals were separated by filtering and were then washed with water. After drying a pale tan solid was obtained which was then dissolved in methylchloroform at reflux temperature, treated with activated charcoal and filtered. The filtrate was cooled to 5° C. and the resulting crystals filtered and dried to give the 4-cyanophenoxyacetonitrile.

후처리

  1. customThe compound of 4-cyanophenoxyacetonitrile was prepared
  2. customresulted in crystal formation
  3. customThe crystals were separated
  4. filtrationby filtering
  5. washwere then washed with water
  6. customAfter drying a pale tan solid
  7. customwas obtained which
  8. temperatureat reflux temperature
  9. filtrationfiltered
  10. filtrationthe resulting crystals filtered
  11. customdried

출처 및 근거

ORD 기록
ord-00053850eedf48998b805479552470f3
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343808

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