Nitric Acid → 1-Chloro-2-fluoro-4-nitro-5-(trifluoromethyl)benzene

HRID 1380717

反応式

HRID 1380717 の反応式
[N+:1]([O-:4])(O)=[O:2].[Cl:5][C:6]1[CH:7]=[C:8]([C:13]([F:16])([F:15])[F:14])[CH:9]=[CH:10][C:11]=1[F:12]>>[Cl:5][C:6]1[C:11]([F:12])=[CH:10][C:9]([N+:1]([O-:4])=[O:2])=[C:8]([C:13]([F:14])([F:15])[F:16])[CH:7]=1

参加物

3

反応物 2

HCID 944Nitric AcidHCID 157153Benzene, 2-chloro-1-fluoro-4-(trifluoromethyl)-

生成物 1

HCID 201633061-Chloro-2-fluoro-4-nitro-5-(trifluoromethyl)benzene

反応条件

温度
40 °C

実験手順

About 500 parts of aqueous nitric acid was added slowly, with stirring, to a reaction vessel containing about 400 parts of 3-chloro-4-fluorobenzotrifluoride. The temperature of the reaction mixture was maintained at about 40° C. during the addition, then raised to about 60° C. and maintained thereat for about 5 hours. The reaction mixture was allowed to settle. The aqueous layer was removed and the organic layer was washed twice with 500 parts of water, treated several times with a saturated solution of sodium bicarbonate, washed with water again, dried over anhydrous magnesium sulfate, and filtered. The filtrate was distilled at reduced pressure to yield 347 parts of 5-chloro-4-fluoro-2-nitrobenzotrifluoride.

後処理

  1. temperatureraised to about 60° C.
  2. temperaturemaintained
  3. customThe aqueous layer was removed
  4. washthe organic layer was washed twice with 500 parts of water
  5. additiontreated several times with a saturated solution of sodium bicarbonate
  6. washwashed with water again
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. distillationThe filtrate was distilled at reduced pressure

出典と根拠

ORDレコード
ord-dc665527b3884235bf2d1dcfd379d226
出典データセット
uspto-grants-1986_04
特許番号
US04582948

関連ノート

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