HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloroethyl chloroformate → 5-Methyl-1,4-oxazepane hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloroethyl chloroformate | HCID 12305 | — |
| Reactant | 4-Benzyl-5-methyl-[1,4]oxazepane | HCID 66718790 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | 5-Methyl-1,4-oxazepane hydrochloride | HCID 66718639 | 78.6% |
Reaction Steps
To a solution of 4-benzyl-5-methyl-[1,4]oxazepane (0.30 g, 1.4 mmol) in 1,2-dichloroethane (3 mL) was added chloroethyl chloroformate (0.56 mL, 7 mmol) at room temperature. The mixture was refluxed for 10 hours and concentrated. The resulting residue was dissolved in methanol (5 mL) and the solution was refluxed for one hour. After concentration, the residual material was triturated, washed with ethyl acetate and collected by filtration to afford 5-methyl-[1,4]oxazepane hydrochloride (0.16 g, 1.1 mmol, 76%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09108957B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-337a7b879283470cba51f99f8306b20f |
| Source note | uspto-grants-2015_08 |