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

HRID 542931

반응식

HRID 542931 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f9a3a7745e0a4edeb479b8851e6d1311
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659834

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