反応 #73465

反応方程式

{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

溶媒

acetone

反応条件

後処理

1. 1
   抽出the reaction mixture was extracted with ethyl acetate three times
2. 2
   抽出The combined organic layer was extracted with brine
3. 3
   乾燥dried over sodium sulphate
4. 4
   その他evaporated to dryness

実験手順

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+).

出典