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Sodium Acetate → HCID 14989225、化合物

HRID 1030920
ノート
印刷プレビュー

反応式

HRID 1030920 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 517045Sodium AcetateHCID 14989224HCID 14989224、化合物

生成物 1

HCID 14989225HCID 14989225、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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;

後処理

  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

出典と根拠

ORDレコード
ord-f813802c5c944f358c466cb593c81eda
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05106973

反応ノート

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