Sodium Hydroxide → 4-chloro-6-methylfuro[3,2-c]pyridine

HRID 1382993노트

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HRID 1382993 반응식
[CH3:1][C:2]1[NH:7][C:6](=O)[C:5]2[CH:9]=[CH:10][O:11][C:4]=2[CH:3]=1.P(Cl)(Cl)([Cl:14])=O.[OH-].[Na+]>>[Cl:14][C:6]1[C:5]2[CH:9]=[CH:10][O:11][C:4]=2[CH:3]=[C:2]([CH3:1])[N:7]=1

참가 물질

4

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 12237176HCID 12237176, 화합물

생성물 1

HCID 122371844-chloro-6-methylfuro[3,2-c]pyridine수율 96%

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온도
100 °C

실험 절차

A mixture of 6-methylfuro[3,2-c]pyridin-4(5H)-one (11.9 g, 0.08 mol) and phosphorus oxychloride (15.2 ml, 0.163 mol) was heated, under a nitrogen atmosphere, at 100° C. for 1.5 hours. The cooled blackish liquid was poured onto crushed ice and the solution made basic with sodium hydroxide solution. The precipitated product was extracted into methylene chloride. This solution was dried over anhydrous sodium sulfate, filtered through a pad of charcoal and evaporated. Pure product was collected by filtration after the residue was triturated with hexane to give 12.9 g (96% yield), mp: 64.5°-66° C.

후처리

  1. additionThe cooled blackish liquid was poured
  2. customonto crushed ice
  3. extractionThe precipitated product was extracted into methylene chloride
  4. dry with materialThis solution was dried over anhydrous sodium sulfate
  5. filtrationfiltered through a pad of charcoal
  6. customevaporated
  7. filtrationPure product was collected by filtration after the residue
  8. customwas triturated with hexane
  9. customto give 12.9 g (96% yield), mp: 64.5°-66° C.

출처 및 근거

ORD 기록
ord-170d0d1eee784ba2989566044e8bbf28
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04808595

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