Acetone → HCID 11263812, compound

Temperature

-50 °C

1.00 g of benzofuran was dissolved in 20 ml of anhydrous tetrahdyrofuran. Thereto was dropwise added 6.2 ml of 1.5 M n-butyllithium hexane solution, in 5 minutes with stirring at -50° C. The mixture was stirred at 0° C. for 30 minutes and then cooled to -50° C. Thereto was added 0.94 ml of acetone. The resulting mixture was stirred at room temperature for 30 minutes. The solvent was removed by distillation under reduced pressure. The residue was mixed with 30 ml of chloroform and 10 ml of water to dissolve the residue. The organic layer was separated, washed with an aqueous saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure to obtain 1.50 g of 2-(1-hydroxy-1-methylethyl)benzofuran as a colorless oily material.

1. stirringThe mixture was stirred at 0° C. for 30 minutes
2. temperaturecooled to -50° C
3. stirringThe resulting mixture was stirred at room temperature for 30 minutes
4. customThe solvent was removed by distillation under reduced pressure
5. additionThe residue was mixed with 30 ml of chloroform and 10 ml of water
6. dissolutionto dissolve the residue
7. customThe organic layer was separated
8. washwashed with an aqueous saturated sodium chloride solution
9. dry with materialdried over anhydrous magnesium sulfate
10. customThe solvent was removed by distillation under reduced pressure

ORD record

ord-50d4dd9339974c4cb058762bf2b866e5

Source dataset

uspto-grants-1992_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05166204