تفاعل #162355
ord-dd94339dac984d52b15bbb10543adaaf
معادلة التفاعل
المتفاعلات
الكواشف
ظروف التفاعل
المعالجة
- 1درجة الحرارةwas heated
- 2درجة الحرارةat reflux for 20 h
- 3درجة الحرارةThe reaction mixture was cooled
- 4درجة الحرارةThe reaction mixture was cooled
- 5تركيزThe reaction mixture was concentrated under reduced pressure
- 6استخلاصthe resulting matterial was extracted with diethyl ether (3×)
- 7تجفيفdried over magnesium sulfate
- 8ترشيحfiltered
- 9تركيزconcentrated under reduced pressure to a tan oil (2.99 g)
- 10أخرىby purified by silica gel column chromatography (5% to 100% gradient of methanol in chloroform as eluant)
الإجراء التجريبي
A mixture of 1,2-diethyl 4-[4-[5-(2,6-difluorophenyl)-4,5-dihydro-3-isoxazolyl]-2-thiazolyl]tetrahydro-1,2-pyridazinedicarboxylate (i.e. the product of Step G) (4.09 g, 0.0083 mol) and potassium hydroxide (2.32 g, 0.0414 mol) in ethanol (50 mL) and water (5 mL) was heated at reflux for 20 h. The reaction mixture was cooled, acidified by the addition of concentrated hydrochloric acid, and then warmed to about 70° C. for 10 minutes. The reaction mixture was cooled, neutralised by the addition of sodium bicarbonate. The reaction mixture was concentrated under reduced pressure and the resulting matterial was extracted with diethyl ether (3×), dried over magnesium sulfate, filtered and concentrated under reduced pressure to a tan oil (2.99 g). The oil was adsorbed onto Celite® (diatomaceous filter aid), and then by purified by silica gel column chromatography (5% to 100% gradient of methanol in chloroform as eluant) to provide the title compound (1.275 g).