تفاعل #46174

ord-3b200dad4b06471d9b74686d147c1eb5

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe mixture was reacted for 1 hour at 70° C.
  2. 2
    غسيلwashed with brine
  3. 3
    استخلاصThe organic layer was extracted with ethyl acetate
  4. 4
    تجفيفdried over anhydrous sulfonate sulfate
  5. 5
    تركيزconcentrated
  6. 6
    أخرىthe resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9)

الإجراء التجريبي

3-Phenyl-6-(3-phenylpropyloxy)-1-oxo-1H-indene-2-carboxylate ethyl ester (1.65 g, 4.0 mmol) prepared in (Step 5) of Example 1 was dissolved in methanol (160 ml) and p-toluene sulfonic acid (228 mg, 1.2 mmol) was added thereto. The mixture was reacted for 1 hour at 70° C., and then washed with brine. The organic layer was extracted with ethyl acetate, dried over anhydrous sulfonate sulfate, concentrated, and the resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9) to obtain the title compound (yield 75.3%) as a red solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741323B2uspto-grants-2010_06