反応 #71791

反応方程式

Benzyl cis(±)-[1-(1H-imidazol-1-ylthiocarbonyl)-3-methoxypiperidin-4-yl]-carbamate

ammonia methanol

→

title compound

収率 67.4%

Benzyl cis(±)-(1-carbamothioyl-3-methoxypiperidin-4-yl)-carbamate

収率 67.4%

溶媒

Brine

THF

反応条件

後処理

1. 1
   抽出followed by extraction with ethyl acetate
2. 2
   乾燥The organic layer was dried over anhydrous sodium sulfate
3. 3
   濃縮concentrated under reduced pressure
4. 4
   ろ過The precipitated solid was collected by filtration

実験手順

Benzyl cis(±)-[1-(1H-imidazol-1-ylthiocarbonyl)-3-methoxypiperidin-4-yl]-carbamate obtained in Example (64a) (about 1.36 mmol) was dissolved in THF (2 mL). A 2 N ammonia/methanol solution (10 mL) was added, and the mixture was stirred for 42 hours. Brine was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The precipitated solid was collected by filtration to obtain 296.5 mg of the title compound as a white solid (67%).

出典