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Sodium Phosphate, Dibasic → HCID 20435948, 화합물

HRID 1154054
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HRID 1154054 반응식
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]
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4

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HCID 24203Sodium Phosphate, DibasicHCID 204359472-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid

생성물 1

HCID 20435948HCID 20435948, 화합물수율 72.3%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-83caaa74b49243c0bf428075d0915044
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04487929

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