تفاعل #742258

ord-9df67d382ae748b7becc42bb30fa3dda

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter complete addition the reaction mixture
  2. 2
    ترشيحThe reaction mixture was filtered
  3. 3
    أخرىevaporated to dryness
  4. 4
    درجة الحرارةThe solution was cooled in the refrigerator overnight
  5. 5
    ترشيحfiltered
  6. 6
    أخرىevaporated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: USRE043006E1uspto-grants-2011_12