HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 19917419, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | HCID 19917414 | HCID 19917414 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 19917419 | HCID 19917419 | 70% |
Reaction Steps
3,4-Dihydro-4-amino-2,2-dimethyl-6-(nonafluorobutyl)sulfonyl-2H-1,4-benzoxazine (0.46 g) was dissolved in 5 ml of pyridine, followed by the dropwise addition of 0.12 ml of methyl chloroformate under ice cooling and stirring. After the reaction mixture was stirred for 15 hours at room temperature, the reaction mixture was added with 10% hydrochloric acid and then extracted twice with chloroform. The combined chloroform layer was washed with water and with saturated brine and was then dried over magnesium sulfate. The solvent was distilled off and the residue was purified by chromatography on a silica gel column, whereby 0.77 g of Compound No. 53 was obtained (yield: 70 %).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05440036 |
| Source dataset | uspto-grants-1995_08 |
| ORD ID | ord-6836d783f97b4a71afd7866d24941958 |
| Source note | uspto-grants-1995_08 |