تفاعل #157811
ord-1ddef37346744936946e7026649bb908
معادلة التفاعل
المتفاعلات
ظروف التفاعل
المعالجة
- 1ترشيحthe insoluble matter was filtered off through celite
- 2استخلاصfollowed by extraction with ethyl acetate
- 3تجفيفThe organic layer was dried over anhydrous magnesium sulfate
- 4ترشيحfiltered
- 5تركيزThe filtrate was concentrated under reduced pressure
- 6أخرىThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:50→0:100)
الإجراء التجريبي
1,4-Dioxane (4 mL) and water (0.4 mL) were added to a mixture of (5R)-5-[(Z)-2-bromo-2-(5-cyclopropyl-6-methoxypyridin-2-yl)ethenyl]pyrrolidin-2-one obtained in Reference Example 4-24 (170 mg), 4-chlorophenylboronic acid (160 mg), tris(dibenzylideneacetone) dipalladium (45 mg), tri(2-furyl)phosphine (69 mg) and cesium carbonate (492 mg), and the mixture was stirred at 90° C. for 2.5 hours. Water and ethyl acetate were added to the reaction solution and the insoluble matter was filtered off through celite, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:50→0:100) to give (5R)-5-[(E)-2-(4-chlorophenyl)-2-(5-cyclopropyl-6-methoxypyridin-2-yl)ethenyl]pyrrolidin-2-one as a crude product (250 mg).