HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloroethyl chloroformate → HCID 66975154, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Reactant | HCID 66975148 | HCID 66975148 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66975154 | HCID 66975154 | 94.4% |
Reaction Steps
To a solution of (6RS,7SR)-4-benzyl-7-({[tert-butyl(dimethyl)silyl]oxy}methyl)-6-(3,4-dichlorophenyl)-1,4-oxazepane (250 mg) in acetonitrile (1.5 mL) was added 1-chloroethyl chloroformate (0.0786 mL), and the mixture was stirred at room temperature for 1.5 hr. The solvent was evaporated under reduced pressure. To the residue was added methanol (1.5 ml), and the reaction mixture was stirred at 60° C. for 3 hr. The solvent was evaporated under reduced pressure. The residue was solidified with diisopropyl ether, and the obtained crude crystals were recrystallized from ethanol/ether/water to give the title compound (76.8 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722662B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-5df39f6e2bf54533b2102a212fabd748 |
| Source note | uspto-grants-2014_05 |