反応 #2286356

反応方程式

cyclohexylmethylmagnesium chloride

tert-butyl 4-{4-[methoxy(methyl)carbamoyl]-1,3-thiazol-2-yl}piperidine-1-carboxylate

ammonium chloride

→

tert-Butyl 4-[4-(cyclohexylacetyl)-1,3-thiazol-2-yl]piperidine-1-carboxylate

溶媒

diethyl ether

tetrahydrofuran

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture was then stirred at room temperature for one hour
2. 2
   その他the aqueous phase was separated off
3. 3
   抽出After extraction of the aqueous phase with ethyl acetate
4. 4
   乾燥the combined organic phases were dried over sodium sulphate
5. 5
   その他the solvent was removed under reduced pressure

実験手順

Under argon and at −78° C., cyclohexylmethylmagnesium chloride 0.5M in diethyl ether (2.7 ml) was added dropwise to a solution of tert-butyl 4-{4-[methoxy(methyl)carbamoyl]-1,3-thiazol-2-yl}piperidine-1-carboxylate (480 mg) in tetrahydrofuran (5 ml). The reaction mixture was stirred at −78° C. for one hour. The reaction mixture was then stirred at room temperature for one hour. Saturated ammonium chloride solution was then added to the reaction mixture, and the aqueous phase was separated off. After extraction of the aqueous phase with ethyl acetate, the combined organic phases were dried over sodium sulphate and the solvent was removed under reduced pressure. This gave tert-butyl 4-[4-(cyclohexylacetyl)-1,3-thiazol-2-yl]piperidine-1-carboxylate (335 mg).

出典