HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → (-)-(cis)-7-bromo-8,14-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 | Dichloromethane | HCID 6344 | — |
| Reactant | (4R)-2-Hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinan 2-oxide | HCID 9829482 | — |
| Reactant | 7-bromo-8,14-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine | HCID 67358639 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | (-)-(cis)-7-bromo-8,14-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 67360816 | 27% |
Reaction Steps
Preparation analogous to Example 5, step i, from 2.2 g, (5.77 mmol) of (±)-(cis)-(7-bromo-8,14-difluoro-1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine, 0.7 g, (2.88 mmol) of (+)-phencyphos, CH2Cl2 (100 mL), ethanol (5 mL) and 2-butanone (50 mL). Recrystallization gave the title compound (0.8 g, 27%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989442B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-ff51b3cfd01d4802af0f3801c8435720 |
| Source note | uspto-grants-2011_08 |