Hydrochloric Acid → 2-(Fluoro-dichloro-methyl)-8-methyl-4-chloro-quinoline

HRID 542931

反応式

HRID 542931 の反応式
[Cl:1][C:2]([Cl:16])(Cl)[C:3]1[CH:12]=[C:11]([Cl:13])[C:10]2[C:5](=[C:6]([CH3:14])[CH:7]=[CH:8][CH:9]=2)[N:4]=1.[Sb](Cl)(Cl)(Cl)(Cl)Cl.[Sb](F)(F)(F)(F)[F:24].Cl>ClCCl>[F:24][C:2]([Cl:16])([Cl:1])[C:3]1[CH:12]=[C:11]([Cl:13])[C:10]2[C:5](=[C:6]([CH3:14])[CH:7]=[CH:8][CH:9]=2)[N:4]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 24294Antimony pentachlorideHCID 24557Antimony pentafluorideHCID 156222554-Chloro-8-methyl-2-(trichloromethyl)quinoline

生成物 1

HCID 156222562-(Fluoro-dichloro-methyl)-8-methyl-4-chloro-quinoline

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3.0 g of 2-trichloromethyl-8-methyl-4-chloro-quinoline are dissolved in 45 ml of dry dichloromethane and under intense stirring 1.5 ml of antimony-penta-chloride and 1.0 ml of antimony-penta-fluoride are added by dropping at a temperature of -5° to 0° C. The mixture is stirred at this temperature for 4 hours and allowed to stand at room temperature for 48 hours. 6 ml of icy concentrated hydrochloric acid are added, the precipitate is filtered, washed with some dichloromethane, the filtrate is separated, dried, filtered and evaporated. 2.1 g solid product are obtained which is recrystallized from heptane: 1.9 g of a yellowish crystalline substance, 68.2%, m.p.: 90°-94° C.

後処理

  1. additionare added
  2. customby dropping at a temperature of -5° to 0° C
  3. waitto stand at room temperature for 48 hours
  4. filtrationthe precipitate is filtered
  5. washwashed with some dichloromethane
  6. customthe filtrate is separated
  7. customdried
  8. filtrationfiltered
  9. customevaporated

出典と根拠

ORDレコード
ord-f9a3a7745e0a4edeb479b8851e6d1311
出典データセット
uspto-grants-1987_04
特許番号
US04659834

関連ノート

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