HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 10753523, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 6-Chloro-3,4-dihydro-2H-benzo[b][1,4]oxazine-8-carboxylic acid | HCID 10608651 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 10753523 | HCID 10753523 | 65.2% |
Reaction Steps
A solution of 10 g of 6-chloro-3,4-dihydro-2H-1,4-benzoxazine-8-carboxylic acid and 6.5 ml of triethylamine in 100 ml of chloroform was cooled, and 4.4 g of acetyl chloride was added thereto with stirring. The resulting mixture was stirred at room temperature for 2 hours. To the liquid reaction mixture were added an aqueous solution of sodium hydrogen carbonate and chloroform, and the resulting organic layer was separated, washed with water, and then dried with magnesium sulfate. The solvent was distilled off under reduced pressure, thereby obtaining 7.8 g of 4-acetyl-6-chloro-3,4-dihydro-2H-1,4-benzoxazine-8-carboxylic acid. Melting point: 76°-77° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05185333 |
| Source dataset | uspto-grants-1993_02 |
| ORD ID | ord-017b71274f0e4c449f3f5ba9ab26b240 |
| Source note | uspto-grants-1993_02 |