Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 67279638 | HCID 67279638 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67279743 | HCID 67279743 | 69% |
Reaction Steps
To a solution of the compound (0.26 g) obtained in step 1 and Et3N (0.21 mL) in THF (10 mL) was added methyl chloroformate (0.12 mL) at 0° C., and the mixture was stirred at 0° C. for 1 hr. The reaction mixture was poured into water, and the resultant product was extracted with ethyl acetate. The organic layer was washed with saturated aqueous ammonium chloride solution and brine and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (solvent gradient; 10→50% ethyl acetate/hexane) to give tert-butyl 8-[4-(methoxycarbonyl)piperazin-1-yl]-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (0.21 g, 69%) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08158617B2 |
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| Source dataset | uspto-grants-2012_04 |
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| ORD ID | ord-daa508ca8eed48b58851f797737a3b58 |
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| Source note | uspto-grants-2012_04 |
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