Phosphorus oxychloride → HCID 86036623, compound

Participants

Reaction Steps

Preparation D11, Step 2: 2-butyl-6-(trifluoromethyl)-quinazolin-4-ol (100 mg, 0.37 mmol, 1 eq) and phosphorus oxychloride (3.00 mL, 3.22 mmol, 87 eq) were mixed at room temperature under nitrogen then refluxed for 3 hours. The reaction was stripped 3 times from methylene chloride. The residue was dissolved in methylene chloride (25 mL) and rinsed 3 times with saturated sodium bicarbonate (25 mL), 1× with water (25 mL). The organic layer was dried (sodium sulfate) and stripped to give 2-butyl-4-chloro-6-(trifluoromethyl)quinazoline (130 mg) as a tan solid. LCMS of a an analytical sample prepared in MeOH detects (M-Cl+OMe)+=285.24.

Provenance & Evidence