تفاعل #461511

ord-60c044af6ebe4e6db57b64cd9b21aca0

ظروف التفاعل

درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAir was then evacuated from autoclave
  2. 2
    workup.ADDITIONcarbon monoxide (30 bar) and ethene (20 bar) were added
  3. 3
    أخرىThe autoclave was then sealed
  4. 4
    أخرىAfter a reaction time of 5 hours, a sample of the contents of the autoclave was withdrawn

الإجراء التجريبي

A 250 ml stainless steel, magnetically stirred autoclave was filled with 0.1 mmol palladium(II)acetate, 5 mmol bisphenyl(2-pyridyl)phosphine, 4 mmol p-toluenesulfonic acid, 40 ml (500 mmol) pyridine, 20 ml methanol and 5 g paraformaldehyde. Air was then evacuated from autoclave, and then carbon monoxide (30 bar) and ethene (20 bar) were added. The autoclave was then sealed and heated to a temperature of 110° C. After a reaction time of 5 hours, a sample of the contents of the autoclave was withdrawn and analyzed by gas liquid chromatography. Two products were found; methoxymethylpropionate, which had been formed with a selectivity of 10%, and methylpropionate, which had been formed with a selectivity of 90%. The mean reaction rate was calculated to be 200 mol ethene/gram atom Pd/hour.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05166411uspto-grants-1992_11