تفاعل #2286303
ord-dd4841b692e048c9ab4c4a6255394cc5
معادلة التفاعل
المتفاعلات
الكواشف
ظروف التفاعل
المعالجة
- 1درجة الحرارةAt this time, the reaction mixture was cooled to room temperature
- 2تركيزwas concentrated under vacuum
- 3workup.ADDITIONThe resulting residue was diluted with methylene chloride (25 mL)
- 4غسيلwas washed with water (10 mL)
- 5أخرىThe organic layer was separated
- 6غسيلwas washed with a saturated aqueous sodium bicarbonate solution (10 mL)
- 7استخلاصextracted with methylene chloride (10 mL)
- 8تجفيفdried with sodium sulfate
- 9ترشيحfiltered
- 10تركيزconcentrated
- 11أخرىdried under high vacuum overnight
الإجراء التجريبي
A solution of 2-[3,5-dichloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-phenyl]-ethanol (17) (500 mg, 1.38 mmol) in glacial acetic acid (5 mL) was treated with sodium acetate (230 mg, 2.8 mmol) and heated to 114° C. for 24 h. At this time, the reaction mixture was cooled to room temperature and was concentrated under vacuum. The resulting residue was diluted with methylene chloride (25 mL) and was washed with water (10 mL). The organic layer was separated and was washed with a saturated aqueous sodium bicarbonate solution (10 mL). The waters layers were combined and extracted with methylene chloride (10 mL). The organic layers were combined and dried with sodium sulfate, filtered, concentrated and dried under high vacuum overnight to afford acetic acid 2-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-yloxy)-phenyl]-ethyl ester (34) (531 mg, 100%) as a white solid; LRMS for C17H18Cl2N2O4 (M+) m/z=385 Molecular Weight=385.2500; Exact Mass=384.0644