反応 #742258

反応方程式

3-[2-(tert-Butyl-dimethyl-silanyloxy)-phenyl]-acrylic acid tert-butyl-dimethyl-silyl ester

oxalyl chloride

→

3-[2-(tert-Butyl-dimethyl-silanyloxy)-phenyl]-acryloyl chloride

溶媒

CH2Cl2

反応条件

後処理

1. 1
   workup.ADDITIONAfter complete addition the reaction mixture
2. 2
   ろ過The reaction mixture was filtered
3. 3
   その他evaporated to dryness
4. 4
   温度The solution was cooled in the refrigerator overnight
5. 5
   ろ過filtered
6. 6
   その他evaporated

実験手順

To a 0° C. cold solution of 6.3 g of 3-[2-(tert-Butyl-dimethyl-silanyloxy)-phenyl]-acrylic acid tert-butyl-dimethyl-silyl ester and 8 drops of DMF in 15 ml of CH2Cl2 was added dropwise 2.0 ml of oxalyl chloride. After complete addition the reaction mixture was allowed to warm to room temperature and stirring was continued for 60 h. The reaction mixture was filtered, evaporated to dryness and taken up in MTBE. The solution was cooled in the refrigerator overnight, filtered and evaporated to yield 4.4 g of 3-[2-(tert-Butyl-dimethyl-silanyloxy)-phenyl]-acryloyl chloride.

出典