反応 #458245

反応方程式

tricyclo[3.3.1.13,7 ]decane-1-carbonyl chloride

3-phenoxybenzyl alcohol

pyridine

→

oily material

収率 98.7%

3-phenoxybenzyl tricyclo[3.3.1.13,7 ]decane-1-carboxylate

収率 98.7%

溶媒

benzene

反応条件

後処理

1. 1
   その他Then the reaction was terminated
2. 2
   その他The resulting pyridine hydrochloride was removed by filtration
3. 3
   洗浄the filtrate was thoroughly washed with 1N hydrochloric acid, 5% sodium carbonate
4. 4
   乾燥saturated saline solution, and dried over sodium sulfate
5. 5
   その他The solvent was removed

実験手順

1 g (5.03 mmol) of tricyclo[3.3.1.13,7 ]decane-1-carbonyl chloride, 1.01 g (5.04 mmol) of 3-phenoxybenzyl alcohol and 0.08 g (10.07 mmol) of anhydrous pyridine were dissolved in 30 ml of anhydrous benzene. The mixture was stirred at room temperature for 66 hours. Then the reaction was terminated. The resulting pyridine hydrochloride was removed by filtration and the filtrate was thoroughly washed with 1N hydrochloric acid, 5% sodium carbonate and then saturated saline solution, and dried over sodium sulfate. The solvent was removed to obtain 1.8 g of an oily material. Purification by column chromatography on silica gel employing a developer consisting of n-hexane and benzene (1:1) gave 1.69 g (yield 93%) of a colorless oily material.

出典