HCID 13144528, 화합물 → HCID 13144530, 화합물

HRID 1154039노트

반응식

HRID 1154039 반응식
C([S:4][CH2:5][C:6]1([CH3:24])[C:21](=[O:22])[N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([O:16]C(C)(C)C)=[O:15])[N:8]2[C:7]1=[O:23])(=O)C>FC(F)(F)C(O)=O>[SH:4][CH2:5][C:6]1([CH3:24])[C:21](=[O:22])[N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([OH:16])=[O:15])[N:8]2[C:7]1=[O:23]

참가 물질

3

반응물 1

HCID 13144528HCID 13144528, 화합물

생성물 1

HCID 13144530HCID 13144530, 화합물수율 43%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 0.71 g of tert.butyl 2-acetylthiomethyl-hexahydro-2-methyl1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate (diastereomer A) in 10 ml of trifluoroacetic acid was left to stand at room temperature for 1 hour. The mixture was evaporated to dryness and the residue was stirred under nitrogen with 50 ml of 50:50 mixture of water and concentrated aqueous ammonia for 2 hours. The mixture was acified to pH 1 with hydrochloric acid, saturated with sodium chloride and extracted with chloroform. The chloroform extracts were dried over sodium sulfate and evaporated. The residue was recrystallized from ethyl acetate/hexane to give 0.22 g (43%) of hexahydro-2-mercaptomethyl-2-methyl-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid (diastereomer A) in the form of white crystals having a melting point of 209°-211° C.

후처리

  1. customThe mixture was evaporated to dryness
  2. extractionextracted with chloroform
  3. dry with materialThe chloroform extracts were dried over sodium sulfate
  4. customevaporated
  5. customThe residue was recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-f0a5c346f7084b82b686ea2488ff5470
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487929

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