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tert.butyl 2-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate → 2-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid

HRID 1154053
ノート
印刷プレビュー

反応式

HRID 1154053 の反応式
[C:1]([S:4][CH2:5][CH:6]1[CH2:21][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:22])(=[O:3])[CH3:2]>FC(F)(F)C(O)=O>[C:1]([S:4][CH2:5][CH:6]1[CH2:21][N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([OH:16])=[O:15])[N:8]2[C:7]1=[O:22])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 20435955tert.butyl 2-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

1.69 of tert.butyl 2-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate (diastereomer A) were treated with 10 ml of trifluoroacetic acid at room temperature for 2 hours. The solution was evaporated and the residue was re-evaporated with toluene several times. The residue was then crystallized from acetone to give 1.1 g of 2-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]-pyridazine-5-carboxylic acid having a melting point of 166°-168° C. (decomposition).

後処理

  1. customThe solution was evaporated
  2. customthe residue was re-evaporated with toluene several times
  3. customThe residue was then crystallized from acetone

出典と根拠

ORDレコード
ord-6c7a35f1f7544e3bbc0905181ad06b9f
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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