Hydrochloric Acid → HCID 178429711, compound
Reaction equation
[SH-:1].[Na+].Cl[C:4]1[N:9]2[N:10]=[CH:11][C:12]([C:13]([O:15]CC)=[O:14])=[C:8]2[N:7]=[C:6]([CH3:18])[CH:5]=1.Cl.[OH-].[K+]>O>[C:13]([C:12]1[CH:11]=[N:10][N:9]2[C:4]([SH:1])=[CH:5][C:6]([CH3:18])=[N:7][C:8]=12)([OH:15])=[O:14]Participants
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 60 °C
Procedure
To a solution of 19 g of sodium hydrosulfide dissolved in 2 liter of water. 19 g (79 mmole) of 7-chloro-3-ethoxycarbonyl-5-methylpyrazolo[1,5-a]pyrimidine was added and stirred at 60° C. for 1 hour. 1he pH of the mixture was adjusted to about 2 with 2N hydrochloric acid under ice-cooling and stirring and the crystals precipitated were collected by filtration and washed with water. The crystals obtained were added to a solution containing 20 g of potassium hydroxide and 150 ml of water and stirred at 60° C. for 2 hours. Then, the pH thereof was adjusted to about 2 with 6N hydrochloric acid under ice-cooling and stirring and the crystals precipitated were collected by filtration. The crystals obtained were washed with water and then dried to obtain 15.8 g of the title compound (Yield: 95.6%).
Workup
- temperaturecooling
- stirringstirring
- customthe crystals precipitated
- filtrationwere collected by filtration
- washwashed with water
- customThe crystals obtained
- additionwere added to a solution
- stirringstirred at 60° C. for 2 hours
- temperaturecooling
- stirringstirring
- customthe crystals precipitated
- filtrationwere collected by filtration
- customThe crystals obtained
- washwere washed with water
- customdried
Sources & evidence
- ORD record
- ord-3e17a6972d2e46daa4571cfe4c8cd15a
- Source dataset
- uspto-grants-1990_10
- Patent number
- US04966900
Reaction notes
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