تفاعل #1481716

ord-f7c7484621c94e5babcf1b22b1a2b313

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with ethyl ether
  2. 2
    أخرىThe residue obtained
  3. 3
    أخرىis purified by chromatography (eluent: 7/3 heptane/ethyl acetate)
  4. 4
    أخرىAfter recrystallization from a heptane/ethyl ether mixture
  5. 5
    أخرىa white solid is obtained (0.65 g; yield=61%; m.p.=201° C.)

الإجراء التجريبي

1.1 g (2 mmol) of methyl 4-(8,8-dimethyl-5-p-tolyl-7,8-dihydro-2-naphthylselanylethynyl)-2-hydroxybenzoate (described in Example 5b) are dissolved in 10 ml of tetrahydrofuran, and 0.96 g (24 mmol) of sodium hydroxide is then added. The reaction medium is heated at 100° C. for 14 hours, acidified with 2N hydrochloric acid solution and then extracted with ethyl ether. The residue obtained is purified by chromatography (eluent: 7/3 heptane/ethyl acetate). After recrystallization from a heptane/ethyl ether mixture, a white solid is obtained (0.65 g; yield=61%; m.p.=201° C.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07348449B2uspto-grants-2008_03