HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 44608378, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 66936726 | HCID 66936726 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 44608378 | HCID 44608378 | 103.3% |
Reaction Steps
In a 25 ml flask, (3-chloro-4-methoxy-5-nitro-phenyl)-(2,3-dihydro-pyrido[3,4-b][1,4]oxazin-1-yl)-methanone (176 mg, 0.441 mmol), lithium chloride (42.7 mg, 1.006 mmol), piperazine (65 mg, 0.755 mmol) and N,N-dimethyl formamide (5 ml) were added and stirred at 1000 for 30 minutes. Lithium chloride (42.7 mg, 1.006 mmol) was further added thereto and then stirred at 1000 for 2 hours. After neutralizing with saturated solution of sodium hydrogen carbonate to pH 8 to 9, the mixture was adjusted to pH 6 again by using 1N hydrochloric acid to form solid. The resulting solid was filtered and recrystallized from methanol and tetrahydrofuran to obtain the target compound 36 as yellow solid (153 mg, 91%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394792B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-97f2c3372d5243779ce83136a49e6f5e |
| Source note | uspto-grants-2013_03 |