HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-Dihydro-2H-1,4-benzoxazine → 63169-10-8
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-Dihydro-2H-1,4-benzoxazine | HCID 585096 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | 63169-10-8 | HCID 21859611 | 77.4% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
3,4-Dihydro-2H-benzo[1,4]oxazine (425 mg, 3.148 mmol) was dissolved in HCl (3N) at 0° C., and stirred for 5 min. at 0° C. A solution of sodium nitrite (217 mg, 3.148 mmol) in water was added at the same temperature, and the reaction mixture stirred at 0° C. for 1 h. After completion of reaction, water was added and the mixture extracted with DCM. The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure, to give 400 mg desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09193728B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-3528499babf147549e375d59ab7f6117 |
| Source note | uspto-grants-2015_11 |