Nitric Acid → 106969-10-2

HRID 2309316ノート

反応式

HRID 2309316 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 13961080106969-10-2収率 89.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ab77e6f4ff46453aae01bba6b1af6565
出典データセット
uspto-grants-1987_09
特許番号
US04695312

反応ノート

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