Hydrochloric Acid → 3-(3-Fluorobenzyl)pyridine

HRID 1904641노트

반응식

HRID 1904641 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][CH:15]=1)[C:5]([C:7]1[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=1)=O.Cl>[Zn].Cl[Hg]Cl.O>[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][CH:15]=1)[CH2:5][C:7]1[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=1

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 129300293-(3-Fluorobenzoyl)pyridine

생성물 1

HCID 200378593-(3-Fluorobenzyl)pyridine수율 29.2%

시약·촉매·용매 3

HCID 23994Zinc촉매2회HCID 24085Mercuric Chloride촉매HCID 962Water용매

실험 절차

Zinc amalgam prepared from zinc (41 g) and HgCl2 (4.1 g) was stirred in a mixture of 3-(3-fluorobenzoyl)pyridine (19.0 g, 0.095 mol), H2O (25 ml) and 12 N HCL (60 ml). The resulting mixture was stirred and heated at reflux for 30 hours. Occasionally during the course of the reaction HCl gas was passed through the mixture, and after 20 hours, additional zinc metal (41 g) was added. After 30 hours the reaction mixture was cooled, decanted, made strongly basic with 10% NaOH, and extracted three times with CH2Cl2. The extracts were dried (Na2SO4) and concentrated, and the residue was distilled to yield 5.2 g (29%) of 3-(3-fluorobenzyl)pyridine: bp 100°-110° C./79.99 Nm-2.

후처리

  1. temperatureheated
  2. temperatureat reflux for 30 hours
  3. temperatureAfter 30 hours the reaction mixture was cooled
  4. customdecanted
  5. extractionextracted three times with CH2Cl2
  6. dry with materialThe extracts were dried (Na2SO4)
  7. concentrationconcentrated
  8. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-d1362b05e0554dda92a287c95c7a7e98
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04839371

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