Nitric Acid → 2,4,5-Trifluoro-3-nitrobenzoic acid

HRID 981362ノート

反応式

HRID 981362 の反応式
[F:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[N+:18]([O-])([OH:20])=[O:19]>>[F:1][C:2]1[C:10]([N+:18]([O-:20])=[O:19])=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

4

反応物 3

HCID 944Nitric Acid2 回HCID 1118Sulfuric AcidHCID 5211702,4,5-Trifluorobenzoic acid

生成物 1

HCID 226086252,4,5-Trifluoro-3-nitrobenzoic acid

反応条件

温度
70 °C

実験手順

3.5 g 0.02 mol of 2,4,5-trifluorobenzoic acid are introduced into a mixture of 6.8 ml of concentrated sulphuric acid and 8 ml of 98% strength nitric acid at 5°-10° C., and the mixture is then stirred without cooling. The temperature increases to 70° C. The mixture is heated for 5 hours at 80°-90° C., a further 8 ml of 98% strength nitric acid are added, and the mixture is heated at 80° C. for 2 hours. The mixture is then introduced into 100 ml of ice water, extracted thoroughly with dichloromethane, dried using sodium sulphate and concentrated. The oil remaining crystallizes. It is stirred with light petroleum, and the solid product is filtered off under suction and dried.

後処理

  1. temperaturewithout cooling
  2. temperatureThe mixture is heated for 5 hours at 80°-90° C.
  3. temperaturethe mixture is heated at 80° C. for 2 hours
  4. extractionextracted thoroughly with dichloromethane
  5. customdried
  6. concentrationconcentrated
  7. customThe oil remaining crystallizes
  8. stirringIt is stirred with light petroleum
  9. filtrationthe solid product is filtered off under suction
  10. customdried

出典と根拠

ORDレコード
ord-1ccd943e5fec4e56827231dbd6320179
出典データセット
uspto-grants-1991_02
特許番号
US04990661

反応ノート

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