Methanol → HCID 14989222, 화합물

HRID 981637노트

반응식

HRID 981637 반응식
[Na].Cl[C:3]1[N:8]=[N:7][C:6]([N:9]2[CH2:14][CH2:13][CH:12]([CH2:15][CH2:16][OH:17])[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[CH3:18][OH:19]>>[CH3:18][O:19][C:3]1[N:8]=[N:7][C:6]([N:9]2[CH2:14][CH2:13][CH:12]([CH2:15][CH2:16][OH:17])[CH2:11][CH2:10]2)=[CH:5][CH:4]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 5360545SodiumHCID 149892211-(6-Chloro-3-pyridazinyl)-4-piperidineethanol

생성물 1

HCID 14989222HCID 14989222, 화합물수율 61.5%

실험 절차

5.7 Parts of sodium (in pieces) were added to 86 parts of methanol. After the dropwise addition of 12.1 parts of 1-(6-chloro-3-pyridazinyl)-4-piperidineethanol, the reaction mixture was stirred overnight at reflux temperature. After cooling, the whole was poured into ice water and the product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of methylbenzene and methanol (90:10 by volume) as eluent. The desired fraction was collected and the eluent was evaporated, yielding 7.3 parts (61.5%) of 1-(6-methoxy-3-pyridazinyl)-4-piperidineethanol as a residue (int. 95).

후처리

  1. temperatureat reflux temperature
  2. temperatureAfter cooling
  3. extractionthe product was extracted with dichloromethane
  4. customThe extract was dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by column chromatography over silica gel using
  8. additiona mixture of methylbenzene and methanol (90:10 by volume) as eluent
  9. customThe desired fraction was collected
  10. customthe eluent was evaporated

출처 및 근거

ORD 기록
ord-052d8533d4724ed88b8cfd26b9e3730d
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04992433

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