Reacción #1969

ord-4f295b3d715849a297bcad06075e2348

Ecuación de reacción

CC(COC1CCCCO1)c1ncc(F)c(Cl)c1F
product
CC(COC1CCCCO1)c1ncc(F)c(Cl)c1F
4-Chloro-3,5-difluoro-2-(1-(2-tetrahydropyranyl)oxy-2-propyl)pyridine
O
water
CC(=O)O
acetic acid
CC(CO)c1ncc(F)c(Cl)c1F
title compound
CC(CO)c1ncc(F)c(Cl)c1F
4-Chloro-3,5-difluoro-2-(1-hydroxy-2-propyl)pyridine

Disolventes

Condiciones de reacción

Temperatura
45°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe THF is removed under reduced pressure
  2. 2
    Extracciónis then extracted with methylene chloride
  3. 3
    SecadoThe organic layer is dried over anhydrous sodium sulfate
  4. 4
    Filtraciónfiltered
  5. 5
    Concentraciónconcentrated in vacuo

Procedimiento

The product of Step 1 is dissolved in 200 mL of 2:1 THF:water and to this solution is added 6 mL of acetic acid. The reaction mixture is heated at 45° C. for approximately 5 hours. The THF is removed under reduced pressure and the aqueous reaction mixture is adjusted to a pH in the range of 8 to 9 with 10% sodium carbonate and is then extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to afford the title compound.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05726182uspto-grants-1998_03