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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Acetate → HCID 14989225, 화합물

HRID 981639
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HRID 981639 반응식
Cl[C:2]1[N:7]=[N:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][CH2:16][OH:17])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C([O-])(=[O:20])C.[Na+]>C(O)(=O)C>[OH:17][CH2:16][CH2:15][CH2:14][CH:11]1[CH2:12][CH2:13][N:8]([C:5]2[CH:4]=[CH:3][C:2](=[O:20])[NH:7][N:6]=2)[CH2:9][CH2:10]1
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참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 14989224HCID 14989224, 화합물

생성물 1

HCID 14989225HCID 14989225, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 6 parts of 1-(6-chloro-3-pyridazinyl)-4-piperidinepropanol, 1.9 parts of sodium acetate and 150 parts of acetic acid was stirred for 4 hours at reflux temperature. The reaction mixture was evaporated and the residue was taken up in 200 parts of a hydrochloric acid solution 10%. After stirring for 1 hour at reflux temperature, the whole was evaporated. The residue was taken up in water and treated with ammonium hydroxide. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated, yielding a first fraction of 6-[4-(3-hydroxypropyl)-1-piperidinyl]-3(2H)-pyridazinone; From the remaining aqueous layer, the precipitated product was filtered off and crystallized from 2-propanol. The product was filtered off and dried at 60° C., yielding a second fraction of the desired intermediate.

후처리

  1. temperatureat reflux temperature
  2. customThe reaction mixture was evaporated
  3. stirringAfter stirring for 1 hour
  4. temperatureat reflux temperature
  5. customthe whole was evaporated
  6. additiontreated with ammonium hydroxide
  7. extractionThe product was extracted with dichloromethane
  8. customThe extract was dried
  9. filtrationfiltered
  10. customevaporated

출처 및 근거

ORD 기록
ord-15f9105fed3f4bebb63ca5bff91ee453
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04992433

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