Hydrazine hydrate (1:1) → HCID 18707265, compound
Reaction equation
C([O:3][C:4]([C:6]1[N:7]=[C:8]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:23][CH3:24])=[C:18]([O:25][CH2:26][CH3:27])[CH:17]=2)[S:9][C:10]=1[C:11](OCC)=[O:12])=O)C.O.[NH2:29][NH2:30]>C(O)C>[CH2:26]([O:25][C:18]1[CH:17]=[C:16]([C:8]2[S:9][C:10]3[C:11](=[O:12])[NH:30][NH:29][C:4](=[O:3])[C:6]=3[N:7]=2)[CH:21]=[CH:20][C:19]=1[O:22][CH2:23][CH3:24])[CH3:27]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 130 °C
Procedure
In 4 ml of ethanol was suspended 1 g of 4,5-diethoxycarbonyl-2-(3,4-diethoxyphenyl)thiazole. Thereto was added 2 ml of hydrazine hydrate. The mixture was sealed in a tube and heated at 130° C. for 48 hours. After cooling, the resulting crystals were collected by filtration, washed with ethanol, dried and recrystallized from dimethylformamide to obtain 220 mg of 2-(3,4-diethoxyphenyl)-5,6-dihydrothiazolo[4,5-d]pyridazine-4,7-dione.
Workup
- customThe mixture was sealed in a tube
- temperatureAfter cooling
- filtrationthe resulting crystals were collected by filtration
- washwashed with ethanol
- customdried
- customrecrystallized from dimethylformamide
Sources & evidence
- ORD record
- ord-becb1bccdb34490880f6a97142dd969b
- Source dataset
- uspto-grants-1997_10
- Patent number
- US05677319
Reaction notes
Loading…