HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 178452593, compound → HCID 86683598, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 178452593 | HCID 178452593 | — |
| Solvent | 1,1,1-Trimethoxybutane | HCID 123512 | — |
| Product | HCID 86683598 | HCID 86683598 | 90% |
Reaction Steps
A solution of (E)-tert-butyl(1-(4-(2-hydrazono-7-phenyl-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-6-yl)phenyl)cyclobutyl)carbamate (60 mg, 0.124 mmol) in 1,1,1-trimethoxybutane (1 ml) was heated to 150° C. for 15 minutes under microwave irradiation. The resulting reaction mixture was concentrated to dryness under reduced pressure and purified by Biotage silica gel chromatography (gradient 0% to 100% ethyl acetate in n-hexanes) to give the title compound (30 mg, 45%). LCMS (Method A): RT=7.34 min, M+1=538. 1H NMR (500 MHz, CDCl3): 7.80 (1H, s), 7.36-7.32 (5H, m), 7.31-7.27 (2H, m), 7.23-7.19 (2H, m), 5.57 (2H, s), 3.08 (2H, t), 2.55-2.40 (4H, m), 2.15-2.03 (1H, m), 2.00 (2H, q), 1.89-1.77 (1H, m), 1.41-1.29 (9H, br), 1.12 (3H, t).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09221838B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-417a5fec63a647ef9b3c595eae941b63 |
| Source note | uspto-grants-2015_12 |