HCID 13144528、化合物 → HCID 13144530、化合物

HRID 1154039ノート

反応式

HRID 1154039 の反応式
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]

参加物

3

反応物 1

HCID 13144528HCID 13144528、化合物

生成物 1

HCID 13144530HCID 13144530、化合物収率 43%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f0a5c346f7084b82b686ea2488ff5470
出典データセット
uspto-grants-1984_12
特許番号
US04487929

反応ノート

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