تفاعل #822558

ord-5a8b602641844da99519e62c681bec69

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction medium is refluxed for 15 hours
  2. 2
    استخلاصextracted with ethyl acetate
  3. 3
    أخرىThe solid obtained
  4. 4
    غسيلis washed with a heptane/ethyl ether mixture (90/10)
  5. 5
    أخرىpurified by chromatography (eluent: dichloromethane)
  6. 6
    أخرىAn off-white powder is obtained (0.2 g; yield=45%)

الإجراء التجريبي

0.46 g (0.95 mmol) of methyl 4-(8,8-dimethyl-5-p-tolyl-7,8-dihydro-2-naphthylselanylethynyl)benzoate is dissolved in 20 ml of tetrahydrofuran, 2 ml of ethanol and 1 ml of water, and 0.46 g (11 mmol) of lithium hydroxide monohydrate is then added. The reaction medium is refluxed for 15 hours, acidified with 2N hydrochloric acid solution and then extracted with ethyl acetate. The solid obtained is washed with a heptane/ethyl ether mixture (90/10) and then purified by chromatography (eluent: dichloromethane). An off-white powder is obtained (0.2 g; yield=45%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07592478B2uspto-grants-2009_09