HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 58170049, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 58170051 | HCID 58170051 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58170049 | HCID 58170049 | — |
Reaction Steps
360 mg (1.11 mmol) of 6-(2,4-dichlorophenyl)-4-oxo-4,5-dihydropyrazolo[1,5-a]pyrazine-2-carboxylic acid (Example 55A) were initially charged in dichloromethane (30 ml) and DMF (10 ml), and 320 mg (1.67 mmol) of EDC, 225 mg (1.67 mg) HOBt and 407 mg (3.33 mmol) of DMAP were added, followed by 0.5M ammonia in dioxane (2.44 ml, 1.22 mmol). The reaction mixture was stirred at RT for 20 h, the solvent was concentrated, the residue was poured into water (25 ml) and the precipitate was filtered off and washed with water and acetonitrile and dried. Drying gave 260 mg (72% of theory) of the product as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09434731B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-47be18e18b1942dfa48cfc96dabaa46f |
| Source note | uspto-grants-2016_09 |