反応 #4384
ord-cd3f0cac90124ff0adb84e6417ad574b
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度cooling
- 2洗浄the mixture was washed with water
- 3乾燥dried over magnesium sulfate
- 4その他evaporated in vacuo
- 5その他The oily residue was purified by column chromatography on silica gel (60 g)
実験手順
Tosyl chloride (3.81 g) was added to a solution of 3-hydroxy-5-hexyn-2-one (2.24 g) and triethylamine (2.424 g) in methylene chloride (20 ml) under ice-cooling. After being stirred for 2.5 hours, the mixture was washed with water, dried over magnesium sulfate and evaporated in vacuo. The oily residue was purified by column chromatography on silica gel (60 g) using methylene chloride as an eluent to give an oil of 3-tosyloxy-5-hexyn-2-one (2.94 g).