Реакция #742258
ord-9df67d382ae748b7becc42bb30fa3dda
Уравнение реакции
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
Реактанты
Реагенты
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1workup.ADDITIONAfter complete addition the reaction mixture
- 2ФильтрацияThe reaction mixture was filtered
- 3Другоеevaporated to dryness
- 4ТемператураThe solution was cooled in the refrigerator overnight
- 5Фильтрацияfiltered
- 6Другоеevaporated
Методика
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.