반응 #73465

반응 방정식

{1-[8-(4-fluoro-phenyl)-1,4-dioxa-spiro[4.5]dec-8-yl]-butyl}-carbamic acid tert-butyl ester

{1-[8-(4-Fluoro-phenyl)-1,4-dioxa-spiro[4.5]dec-8-yl]-butyl}-carbamic acid tert-butyl ester

hydrochloric acid

sodium bicarbonate

→

( 17 )

{1-[1-(4-Fluoro-phenyl)-4-oxo-cyclohexyl]-butyl}-carbamic acid tert-butyl ester

용매

acetone

반응 조건

후처리

1. 1
   추출the reaction mixture was extracted with ethyl acetate three times
2. 2
   추출The combined organic layer was extracted with brine
3. 3
   건조dried over sodium sulphate
4. 4
   기타evaporated to dryness

실험 절차

1.22 g of {1-[8-(4-fluoro-phenyl)-1,4-dioxa-spiro[4.5]dec-8-yl]-butyl}-carbamic acid tert-butyl ester (16) were dissolved in 42 mL of acetone and 3 mL of 1N hydrochloric acid were added. The mixture was stirred at room temperature until conversion was complete. 40 mL of saturated aqueous sodium bicarbonate solution were added and the reaction mixture was extracted with ethyl acetate three times. The combined organic layer was extracted with brine, dried over sodium sulphate and evaporated to dryness to give 966 mg of crude (17), that was sufficiently pure for further conversion. Rt=1.72 min (Method 5). Detected mass: 308.2 (M-Isobutene+H+).

출처