反应详情

Compound XI (3.00 g, 15 mmol) was heated under reflux with excess POCl3 (25 mL) until no starting material remained (TLC, silic gel, 5% methanol in methylene chloride), then poured over ice, made basic with aqueous sodium hydroxide and the aqueous phase extracted with methylene chloride to isolate the product. The organic phase was dried (MgSO4), filtered, and evaporated to give a residue which was purified by flash column chromatography (silica gel, 5% methanol in methylene chloride) to give 1-chloro-4-methyl-6,7,8,9-tetrahydropyridazino[4,5-b]indolizine XII (3.00 g, 92%)

1. additionpoured over ice
2. extractionthe aqueous phase extracted with methylene chloride
3. customto isolate the product
4. dry with materialThe organic phase was dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customto give a residue which
8. customwas purified by flash column chromatography (silica gel, 5% methanol in methylene chloride)