Hydrochloric Acid → HCID 20436001, compound
Reaction equation
C([S:4][CH2:5][CH2:6][C:7]1([CH3:22])[C:19](=[O:20])[N:10]2[CH2:11][CH:12]=[CH:13][CH:14]([C:15]([O:17]C)=[O:16])[N:9]2[C:8]1=[O:21])(=O)C.Cl>>[SH:4][CH2:5][CH2:6][C:7]1([CH3:22])[C:19](=[O:20])[N:10]2[CH2:11][CH:12]=[CH:13][CH:14]([C:15]([OH:17])=[O:16])[N:9]2[C:8]1=[O:21]Participants
3
Procedure
1.1 g of methyl 2-(2-acetylthioethyl)-2,3,5,8-tetrahydro-2-methyl-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate (diastereomer A) were heated under reflux for 3 hours with 25 ml of 2 M hydrochloric acid. After evaporation, the residue was taken up in dichloromethane, the solution was dried over magnesium sulfate and then evaporated. There was obtained 0.35 g (38%) of 2,3,5,8-tetrahydro-2-(2-mercaptoethyl)-2-methyl-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid (diastereomer A) in the form of a white solid having a melting point of 113°-114° C. (from diethyl ether/petroleum ether).
Workup
- customAfter evaporation
- dry with materialthe solution was dried over magnesium sulfate
- customevaporated
Sources & evidence
- ORD record
- ord-9650124b700747f28cb2082295556d35
- Source dataset
- uspto-grants-1984_12
- Patent number
- US04487929
Reaction notes
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