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Sodium Phosphate, Dibasic → HCID 20435948、化合物

HRID 1154054
ノート
印刷プレビュー

反応式

HRID 1154054 の反応式
C([S:4][CH2:5][CH:6]1[CH2:17][N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([OH:16])=[O:15])[N:8]2[C:7]1=[O:18])(=O)C.P([O-])([O-])(O)=O.[Na+].[Na+]>Cl>[SH:4][CH2:5][CH:6]1[CH2:17][N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([OH:16])=[O:15])[N:8]2[C:7]1=[O:18]
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 24203Sodium Phosphate, DibasicHCID 204359472-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid

生成物 1

HCID 20435948HCID 20435948、化合物収率 72.3%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

1.8 g of 2-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid were heated at 95° C. for 1.5 hours in 2 M hydrochloric acid. The mixture was cooled, the pH was adjusted to 3 by the addition of disodium hydrogen orthophosphate and the aqueous solution was extracted repeatedly with ethyl acetate. The organic extracts were dried over magnesium sulfate and evaporated. After recrystallization of the residue from acetone, there were obtained 1.1 g of hexahydro-2-mercaptomethyl-3-oxo-1H- pyrazolo[1,2-a]pyridazine-5-carboxylic acid having a melting point of 145.5°-147° C.

後処理

  1. temperatureThe mixture was cooled
  2. extractionthe aqueous solution was extracted repeatedly with ethyl acetate
  3. dry with materialThe organic extracts were dried over magnesium sulfate
  4. customevaporated
  5. customAfter recrystallization of the residue from acetone

出典と根拠

ORDレコード
ord-83caaa74b49243c0bf428075d0915044
出典データセット
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04487929

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート