반응 #742258

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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

용매

CH2Cl2

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후처리

1. 1
   workup.ADDITIONAfter complete addition the reaction mixture
2. 2
   여과The reaction mixture was filtered
3. 3
   기타evaporated to dryness
4. 4
   온도The solution was cooled in the refrigerator overnight
5. 5
   여과filtered
6. 6
   기타evaporated

실험 절차

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.

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