تفاعل #2301546

ord-6056f811a1854197b0e3f66582c64b4f

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    workup.WAITat 120° C. for 2 hours
  2. 2
    درجة الحرارةThe reaction mixture was cooled to room temperature
  3. 3
    استخلاصthe mixture was extracted with ethyl acetate
  4. 4
    غسيلThe organic layer was washed with saturated aqueous sodium chloride solution
  5. 5
    تجفيفdried over anhydrous magnesium sulfate
  6. 6
    تركيزconcentrated

الإجراء التجريبي

A mixture of 0.30 g of methyl [3-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-pyridyloxy]acetate (compound a-6), 0.06 g of sodium carbonate, and 3.0 ml of cyclopentanol was stirred at 100° C. for 1.5 hours and then at 120° C. for 2 hours. The reaction mixture was cooled to room temperature and then poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.15 g of cyclopentyl [3-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-pyridyloxy]acetate (compound a-28).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07109148B2uspto-grants-2006_09