HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66936690, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Chloro-4-methoxybenzoyl chloride | HCID 4769299 | — |
| Reactant | 2,3-Dihydro-1H-pyrido[3,4-b][1,4]oxazine | HCID 21961536 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66936690 | HCID 66936690 | 99.8% |
Reaction Steps
In a 10 ml flask, 2,3-dihydro-1H-pyrido[3,4-b][1,4]oxazine (60 mg, 0.441 mmol) and 3-chloro-4-methoxy-benzoyl chloride (108 mg, 0.529 mmol) were dissolved in dichloromethane (3 ml). Triethylamine (0.12 ml, 0.881 mmol) was added thereto and then stirred at room temperature for 2 hours. After neutralizing with 1N hydrochloric acid solution, the mixture was extracted with dichloromethane, and the combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure. The residue was purified by column chromatography on silica eluting with a solvent of ethyl acetate:n-hexane=1:1. The fractions containing the product were collected and evaporated to obtain white solid (134 mg, 99.8%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394792B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-21df6349b9dd40eea122ffbc28de0df0 |
| Source note | uspto-grants-2013_03 |