Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Acetone cardice | HCID 18522661 | — |
| Reactant | HCID 67913256 | HCID 67913256 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10199053 | HCID 10199053 | — |
Reaction Steps
A mixture of 4.5 g (0.015 mole) of 3-(dimethylamino)-5-(4-methylphenyl)pyrazole-4-acetic acid monohydrochloride and 4 ml (0.03 mole) of triethylamine in 75 ml of methylene chloride was stirred under nitrogen until all the solids dissolved, then cooled to -30° C. in a dry ice/acetone batch and treated with 1.7 g (0.0152 mole) of ethyl chloroformate added dropwise through a septum with a syringe and needle. The reaction mixture was cooled to 0° C. with an ice-brine bath and ammonia (5 ml in 10 ml of methylene chloride) was added. The reaction was stirred for 16 hours as it warmed to ambient temperature.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05057534 |
|---|
| Source dataset | uspto-grants-1991_10 |
|---|
| ORD ID | ord-412acffc379845b6a5f6b7c9e8c95266 |
|---|
| Source note | uspto-grants-1991_10 |
|---|