HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 13768694, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-Chloropropionyl chloride | HCID 111019 | — |
| Reactant | 3-Methyl-3,4-dihydro-2H-1,4-benzoxazine | HCID 2763760 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 13768694 | HCID 13768694 | 165.2% |
Reaction Steps
5.35 ml (55 mmoles) of 2-chloropropionyl chloride are added dropwise, at a temperature of 20° to 25° C. and while stirring, to a suspension of 7.5 g (50 mmoles) of 2,3-dihydro-3-methyl-1,4-benzoxazine and 5.8 g (55 mmoles) of sodium carbonate in 120 ml of benzene. The reaction mixture is then stirred at the same temperature for 30 minutes and is then taken up in a mixture of water and ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated. Crystallising the residue from diisopropyl ether gives 19.8 g of 4-(2-chloropropionyl)-2,3-dihydro-3-methyl-1,4-benzoxazine, melting point 88°-90° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04618361 |
| Source dataset | uspto-grants-1986_10 |
| ORD ID | ord-2583bb2b116141ae8619ae631d63abd9 |
| Source note | uspto-grants-1986_10 |