Nitric Acid → 106969-10-2

HRID 2309316노트

반응식

HRID 2309316 반응식
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[Cl:10][C:11]1[CH:16]=[C:15]([F:17])[CH:14]=[CH:13][C:12]=1[O:18][CH:19]([F:21])[F:20]>C(Cl)(Cl)Cl>[Cl:10][C:11]1[C:12]([O:18][CH:19]([F:20])[F:21])=[CH:13][C:14]([N+:1]([O-:4])=[O:2])=[C:15]([F:17])[CH:16]=1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 139610792-Chloro-1-(difluoromethoxy)-4-fluorobenzene

생성물 1

HCID 13961080106969-10-2수율 89.5%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
60 °C

실험 절차

To 21 g of conc. nitric acid was dropwise added 28 g of conc. sulfuric acid at 0° C., and the mixture was heated at 60° C. At intervals of 3 minutes, 10 g of 1-chloro-2-difluoromethoxy-5-fluorobenzene was added in 5 portions to the mixture, which was kept at 60° C. for half an hour. After cooling, the reaction mixture was poured on ice water and shaken with chloroform. The chloroform layer was washed with water, dried and concentrated. The residue was chromatographed on a column of silica gel, eluting with n-hexane-ethyl acetate (100:15 v/v). The eluate was concentrated to give 11 g of the titled compound XII-1.

후처리

  1. customat 0° C.
  2. waitwas kept at 60° C. for half an hour
  3. temperatureAfter cooling
  4. additionthe reaction mixture was poured on ice water
  5. washThe chloroform layer was washed with water
  6. customdried
  7. concentrationconcentrated
  8. customThe residue was chromatographed on a column of silica gel
  9. washeluting with n-hexane-ethyl acetate (100:15 v/v)
  10. concentrationThe eluate was concentrated

출처 및 근거

ORD 기록
ord-ab77e6f4ff46453aae01bba6b1af6565
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04695312

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