تفاعل #46910

ord-d78045a97bc94da69a2c6f2ecb99a3ea

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was removed under reduced pressure
  2. 2
    أخرىthe crude residue was purified by silica gel column (dichloromethane/methyl alcohol 9.75:0.25)
  3. 3
    أخرىto furnish 2.9 g of crude compound 6
  4. 4
    أخرىThe obtained compound was purified by a silica gel open column
  5. 5
    غسيلeluted with CH2Cl2/MeOH (9.5/0.5))

الإجراء التجريبي

4-Carbamoylphenyl 2-(2-methoxynaphthalen-6-yl)-propanoate, 5 (1.80 g, 4.34 mmol) and Lawesson reagent (1.75 g, 4.34 mmol) were dissolved in 130 ml of anhydrous benzene. The reaction was warmed to 60° C. and stirred for 4 h. The solvent was removed under reduced pressure; the crude residue was purified by silica gel column (dichloromethane/methyl alcohol 9.75:0.25) to furnish 2.9 g of crude compound 6. The obtained compound was purified by a silica gel open column and eluted with CH2Cl2/MeOH (9.5/0.5)) giving the pure compound 6 (970 mg, 61% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741359B2uspto-grants-2010_06