HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21098407, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 21098387 | HCID 21098387 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 21098407 | HCID 21098407 | — |
Reaction Steps
To a solution of (3-bromo-phenyl)-(6,7-dimethoxy-5-nitro-quinazolin-4-yl)-amine (0.2 g, 0.49 mmol) (from Example 6, Step A, supra) and NH4Cl (0.26 g, 4.94 mmol) in a mixture of MeOH, H2O and CHCl3 (30 mL, 6:1:1) was added Zn powder (0.64 g, 9.87 mmol). The reaction mixture was stirred at room temperature for 3 hours. The mixture was then filtered, the filtrate was concentrated and then extracted with chloroform (100 mL). The organic layer was separated, dried over Na2SO4, and concentrated. This residue was purified by chromatography using EtOAc/CH2Cl2 /NEt3 (1:1:0.05) as eluent to give the desired N4-(3-bromo-phenyl)-6,7-dimethoxy-quinazoline-4,5-diamine as a yellow gum. (Yield 0.1 g, 54%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07217717B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-2dae9fea763a4eb1a8c53d29e7d1b55f |
| Source note | uspto-grants-2007_05 |