Sulfuric Acid → HCID 23358995、化合物

HRID 2396960ノート

反応式

HRID 2396960 の反応式
[F:1][C:2]1[C:7]([F:8])=[C:6]([Cl:9])[CH:5]=[C:4]([F:10])[C:3]=1[CH3:11].S(=O)(=O)(O)O.[N+:17]([O-])([O-:19])=[O:18].[K+]>>[F:1][C:2]1[C:7]([F:8])=[C:6]([Cl:9])[C:5]([N+:17]([O-:19])=[O:18])=[C:4]([F:10])[C:3]=1[CH3:11]

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 23358997HCID 23358997、化合物

生成物 1

HCID 23358995HCID 23358995、化合物収率 61.9%

反応条件

温度
0 °C

実験手順

To 2,3,6-trifluoro-4-chlorotoluene (0.22 g) is added conc. sulfuric acid (3 ml) and the mixture is cooled to 0° C. Thereto potassium nitrate (0.18 g) is added and the mixture is stirred for 15 minutes under ice-cooling. The reaction mixture is poured into ice-water, extracted with dichloromethane, and the extract is washed with a saturated aqueous solution of sodium hydrogen carbonate, then with water and dried. The solvent is distilled off under reduced pressure to give 2,3,6-trifluoro-4-chloro-5-nitrotoluene (0.17 g).

後処理

  1. temperaturecooling
  2. extractionextracted with dichloromethane
  3. washthe extract is washed with a saturated aqueous solution of sodium hydrogen carbonate
  4. dry with materialwith water and dried
  5. distillationThe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-8928d7dfc45b4116addec2a8a31c2774
出典データセット
uspto-grants-1996_02
特許番号
US05495020

反応ノート

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