反应 #742258

ord-9df67d382ae748b7becc42bb30fa3dda

反应方程式

CC(C)(C)[Si](C)(C)OC(=O)C=Cc1ccccc1O[Si](C)(C)C(C)(C)C
3-[2-(tert-Butyl-dimethyl-silanyloxy)-phenyl]-acrylic acid tert-butyl-dimethyl-silyl ester
O=C(Cl)C(=O)Cl
oxalyl chloride
CC(C)(C)[Si](C)(C)Oc1ccccc1C=CC(=O)Cl
3-[2-(tert-Butyl-dimethyl-silanyloxy)-phenyl]-acryloyl chloride

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE043006E1uspto-grants-2011_12