HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 69054751, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 3,4-Dihydro-2H-1,4-benzoxazine | HCID 585096 | — |
| Reactant | 2-[2-(5-Fluoro-2-methoxyphenyl)-2-methylpropyl]-2-trifluoromethyloxirane | HCID 16099239 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 69054751 | HCID 69054751 | — |
Reaction Steps
A mixture of 2-[2-(5-fluoro-2-methoxyphenyl)-2-methylpropyl]-2-trifluoromethyloxirane (see Example 1) (0.139 g) and 3,4-dihydro-2H-benzo[1,4]oxazine (0.76 g) was dissolved in approximately 5 mL of methylene chloride and 0.55 g of flash silica gel was added. The volatiles were removed in vacuo and the residue was microwaved for 60 seconds at 150° C. and applied to a column of flash silica gel. Elution with EtOAc-hexanes (1:10) and concentration in vacuo of the product-rich fractions provided a residue which was dissolved in diethyl ether. HCl in dioxane was added. The volatiles were removed in vacuo and the residue triturated with diethyl ether. The resulting solid was dried in vacuo to provide the title compound, m.p. 98° C.-99° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07579469B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-dfe380ba5e2a48eb8b773c1863dae4a6 |
| Source note | uspto-grants-2009_08 |