تفاعل #2155663

ord-96ac6f35c69e43759a3cdf9756ec0546

المذيبات

ظروف التفاعل

درجة الحرارة
20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe methanol was removed under reduced pressure
  2. 2
    workup.ADDITIONthe residue was poured into a mixture of 10 ml of water and 15 ml of dichloromethane
  3. 3
    استخلاصThe aqueous phase was extracted with 15 ml of dichloromethane
  4. 4
    استخلاصextracted three times with in each case 15 ml of dichloromethane
  5. 5
    أخرىDrying of the combined organic phases and removal of the solvent under reduced pressure
  6. 6
    أخرىgave 0.207 g (99% of theory) of a brown wax-like solid, melting point 55° C.

الإجراء التجريبي

0.111 g (2.772 mmol) of 2-molar aqueous sodium hydroxide solution was added to 0.200 g (0.554 mmol) of methyl[1-(6-chloropyridazin-3-yl)-5-hydroxy-3-methyl-5-phenyl-4,5-dihydro-1H-pyrazol-4-yl]acetate in 8 ml of methanol, and the mixture was stirred at 20° C. for 1 h. The methanol was removed under reduced pressure and the residue was poured into a mixture of 10 ml of water and 15 ml of dichloromethane. The aqueous phase was extracted with 15 ml of dichloromethane, acidified with concentrated hydrochloric acid (pH=3) and extracted three times with in each case 15 ml of dichloromethane. Drying of the combined organic phases and removal of the solvent under reduced pressure gave 0.207 g (99% of theory) of a brown wax-like solid, melting point 55° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08298994B2uspto-grants-2012_10