반응 #1748583

반응 방정식

ICN

2-Methyl-6,7-dihydro-8H-indeno[5,4-d][1,3]oxazol-8-one

acetone

Acetone

→

title compound

수율 33.0%

2-Methyl-7-(1-methylethylidene)-6,7-dihydro-8H-indeno[5,4-d][1,3]oxazol-8-one

수율 33.0%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was further stirred for 12 hr
2. 2
   여과The reaction solution was filtered
3. 3
   기타the filtrate was evaporated under reduced pressure
4. 4
   기타The residue was purified by silica gel column chromatography (ethyl acetate/hexane=10/90→50/50)

실험 절차

2-Methyl-6,7-dihydro-8H-indeno[5,4-d][1,3]oxazol-8-one (1.87 g, 10.0 mmol), acetone (3.68 mL, 50.0 mmol) and ICN Alumina B (manufactured by ICN, Akt.1, 20 g) were suspended in tetrahydrofuran (50 mL), and the mixture was stirred at 50° C. for 9 hr. Acetone (3.68 mL, 50.0 mmol) was added, and the mixture was further stirred for 12 hr. The reaction solution was filtered, and the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=10/90→50/50) to give the title compound (742 mg, yield 33%).

출처