HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → tert-butyl 7-bromo-2H,3H,4H-pyrido[3,2-b][1,4]oxazine-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 4(tert-Butoxycarbonyl)-3,4-dihydro-2H-pyrido[3,2-b]-1,4-oxazine | HCID 22139145 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | tert-butyl 7-bromo-2H,3H,4H-pyrido[3,2-b][1,4]oxazine-4-carboxylate | HCID 22139026 | 48% |
Reaction Steps
To a solution of 4-(tert-butoxycarbonyl)-3,4-dihydro-2H-pyrido[3,2-b]-1,4-oxazine (2.0 g, 8.46 mmole) in MeOH (40 mL) was added Br2 (0.53 mL, 10.2 mmole) dropwise at 0° C. After 1 hr the mixture was concentrated. The residue was taken up in 1:1 Et2O/hexanes and filtered. The filtrate was concentrated under reduced pressure to give the title compound (1.27 g, 48%) as an oil which solidified under vacuum: 1H NMR (400 MHz, CDCl3) δ 8.10 (s, 1H), 7.33 (s, 1H), 4.25 (m, 2H), 3.92 (m, 2H), 1.54 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07250424B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-ef4076f883f84b41866b988c04c5d51e |
| Source note | uspto-grants-2007_07 |