HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → (-)-(cis)-7-bromo-8,11-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (4S)-2-hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinane 2-oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | (4R)-2-Hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinan 2-oxide | HCID 9829482 | — |
| Reactant | (+/-)-(cis)-7-Bromo-8,11-difluoro-1,3,4,14b-tetrahydro-2h-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine | HCID 67358065 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (-)-(cis)-7-bromo-8,11-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (4S)-2-hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinane 2-oxide | HCID 67358064 | 26.8% |
Reaction Steps
Preparation analogous to Example 5, step i, from (±)-(cis)-7-bromo-8,11-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (30.5 mmol) and (+)-phencyphos (3.7 g, 15.29 mmol) in CH2Cl2 (160 mL), and ethanol (100 mL). Recrystallization gave the title compound (2.55 g, 17%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989442B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-ae9ea876c64b4b1da32a6fcb172605c0 |
| Source note | uspto-grants-2011_08 |