反応 #3043

反応方程式

acetylchloride

hydrochloric acid

2,6-di-t-butylphenol

→

desired subtitled intermediate

1-[3,5-bis(1,1-dimethylethyl) -4-hydroxyphenyl]ethanone

溶媒

methylene chloride

反応条件

後処理

1. 1
   その他The mixture separated into layers which
2. 2
   その他were subsequently separated
3. 3
   洗浄The organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine
4. 4
   その他The organic layer was dried
5. 5
   その他the solvent evaporated

実験手順

Under a nitrogen atmosphere, 6.89 ml of acetylchloride and 14.75 ml of stannic chloride were dissolved in 200 ml of methylene chloride and chilled to -4° C. To this was added 20 g of 2,6-di-t-butylphenol (in 100 ml of methylene chloride) over 10 minutes. The resultant mixture was stirred for 30 minutes at 0° C., then poured into a mixture of 400 ml of ice and 1N hydrochloric acid and stirred. The mixture separated into layers which were subsequently separated. The organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine. The organic layer was dried and the solvent evaporated to give 23.39 g of the desired subtitled intermediate.

出典