تفاعل #73465

معادلة التفاعل

{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

المذيبات

acetone

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe reaction mixture was extracted with ethyl acetate three times
2. 2
   استخلاصThe combined organic layer was extracted with brine
3. 3
   تجفيفdried over sodium sulphate
4. 4
   أخرىevaporated to dryness

الإجراء التجريبي

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+).

المصدر