反応 #2348133

反応方程式

3,7,11-trimethyldodecanol

pyridine

p-toluenesulfonyl chloride

→

3,7,11-trimethyldodecyl tosylate

収率 108.7%

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   workup.ADDITIONAfter the dropwise addition
2. 2
   その他the resulting reaction solution
3. 3
   洗浄was successively washed with 200 ml of water, 200 ml of 2N hydrochloric acid, and 200 ml of a saturated sodium bicarbonate water
4. 4
   乾燥was dried over anhydrous magnesium sulfate
5. 5
   ろ過After the filtration
6. 6
   濃縮the resultant was concentrated

実験手順

Under a nitrogen atmosphere, a solution of 22.8 g (100 mmol) of 3,7,11-trimethyldodecanol and 9.48 g (120 mmol) of pyridine in 200 ml of dry methylene chloride was added dropwise to a solution of 20.96 g (110 mmol) of p-toluenesulfonyl chloride in 100 ml of dry methylene chloride under ice cooling (1 to 2° C.). After the dropwise addition, the resultant was agitated at room temperature overnight, the resulting reaction solution was successively washed with 200 ml of water, 200 ml of 2N hydrochloric acid, and 200 ml of a saturated sodium bicarbonate water, and was dried over anhydrous magnesium sulfate. After the filtration, the resultant was concentrated to obtain 41.6 g of crude 3,7,11-trimethyldodecyl tosylate.

出典