Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 22136471 | HCID 22136471 | — |
| Product | HCID 22136497 | HCID 22136497 | 76% |
Reaction Steps
A mixture of 2-chloro-4-(3-chlorophenyl)-α-(4-chlorophenyl)-α-(1-methyl-1H-imidazol-5-yl)-6-quinazolinemethanol (0.0040 mol), described in International Patent Specification WO 00/39082, in hydrazine (20 ml) and dioxane (40 ml) was stirred at 70° C. for 20 minutes. Saturated sodium chloride solution was added. The mixture was extracted with DCM. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated till dryness. The residue (2.15 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH; 95/5 to 90/10; 70–200 μm). The pure fractions were collected and the solvent was evaporated, yielding 1.5 g (76%) of 4-(3-chlorophenyl)-α-(4-chlorophenyl)-2-hydrazino-α-(1-methyl-1H-imidazol-5-yl)-6-quinazolinemethanol, mp.186° C. (intermediate 11).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07053105B2 |
|---|
| Source dataset | uspto-grants-2006_05 |
|---|
| ORD ID | ord-002dc74ad44549d1873b60f909951546 |
|---|
| Source note | uspto-grants-2006_05 |
|---|