HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59242049, compound → HCID 59242042, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59242049 | HCID 59242049 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 59242042 | HCID 59242042 | — |
Reaction Steps
10% Pd—C (10 mg, 0.0094 mmol) was added to a soln of (2-fluoro-4-methoxy-phenyl)-methyl-(2-methyl-6-nitro-quinazolin-4-yl)-amine (127 mg, 0.371 mmol) in AcOH (3 mL) and this was reacted under 1 atm of hydrogen. After 3 h, the rxn was filtered through a 0.45 μm filter then concentrated. Satd NaHCO3 (10 mL) was added and the product extracted into CHCl3 (2×2 mL). The soln was dried (MgSO4), filtered through a plug of silica with an EtOAc wash then concd to a yellow crystalline solid (104 mg; 90%). 1H NMR (CDCl3) δ 7.61 (d, J=8.8 Hz, 1H), 7.05-6.99 (m, 2H), 6.73 (dd, J=2.8, 12 Hz, 1H), 6.66 (ddd, J=1.2, 3.2, 8.8 Hz, 1H), 6.18 (d, J=2.4 Hz, 1H), 3.82 (s, 3H), 3.51 (s(br), 2H), 3.50 (s, 3H), 2.69 (s, 3H); LC-MS (ESI+; 313 ([M+H]+)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309562B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-8c2355e608ef4c958e15aa348f473b35 |
| Source note | uspto-grants-2012_11 |