Реакция #2275727

ord-9ab9905baa1c470ca236d29b40e48295

Уравнение реакции

O=c1ccccn1C1CCC2(CC1)OCCO2
1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-pyridin-2-one
Cl
HCl
O=C([O-])O.[Na+]
sodium bicarbonate
O=C1CCC(n2ccccc2=O)CC1
title compound
O=C1CCC(n2ccccc2=O)CC1
1-(4-Oxo-cyclohexyl)-1H-pyridin-2-one

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe solvent was removed in vacuo and residue
  2. 2
    Другоеpartitioned between ethyl acetate and water
  3. 3
    ПромывкаThe organic layer was washed with brine
  4. 4
    Сушкаdried over anhydrous Na2SO4
  5. 5
    Фильтрацияfiltered
  6. 6
    Концентрированиеconcentrated

Методика

A solution of 1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-pyridin-2-one (as prepared in the previous step, ˜300 mg, 1.28 mmol)) in acetone (10 mL) was treated with 1N HCl (2 mL) at room temperature for 4 hours. The reaction was worked up with saturated sodium bicarbonate to adjust the pH to neutral. The solvent was removed in vacuo and residue partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered, concentrated to afford the title compound as white solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08324186B2uspto-grants-2012_12