Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 9-Fluoro-5,6-dihydro-2,3-diiodoimidazo[1,2-d][1,4]benzoxazepine | HCID 58204914 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Ammonium Chloride | HCID 25517 | — |
| Product | HCID 58204465 | HCID 58204465 | 88% |
Reaction Steps
9-fluoro-2,3-diiodo-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine (1.24 g, 2.74 mmol) was dissolved in tetrahydrofuran (25 mL, 310 mmol) and cooled to −78° C. in a dry ice/acetone bath. Added 3.0 Methylmagnesium bromide in ether (1.37 mL and allowed the reaction to warm up to −40° C. and stir for 4 hours. Complete by LCMS. Diluted with 100 mL of saturated ammonium chloride and extracted with ethyl acetate. Dried over magnesium sulfate, concentrated in vacuo and purified by flash chromatography on the ISCO 0-40% ethyl acetate in hexanes to give 9-fluoro-2-iodo-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine (0.794 g, 88% yield)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08343955B2 |
|---|
| Source dataset | uspto-grants-2013_01 |
|---|
| ORD ID | ord-ddaa375f31894f7c8c869057e8f267ce |
|---|
| Source note | uspto-grants-2013_01 |
|---|
