Reacción #490739

Ecuación de reacción

2,2-difluoroethanol

methyl 5-fluoro-2-nitrobenzoate

NEt3

2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane

→

expected product

Rendimiento 92.5%

Methyl 5-(2,2-difluoroethoxy)-2-nitrobenzoate

Rendimiento 92.5%

Disolventes

THF

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe solvent is evaporated under reduced pressure
2. 2
   workup.ADDITIONWater is added
3. 3
   Extracciónextraction
4. 4
   LavadoThe extract is washed with a 1N aqueous HCl solution, with water
5. 5
   SecadoIt is dried over MgSO4
6. 6
   Filtraciónfiltered
7. 7
   Otrothe solvent is evaporated under reduced pressure

Procedimiento

8.53 g of 2,2-difluoroethanol are added to a solution of 17.31 g of methyl 5-fluoro-2-nitrobenzoate, 9.64 g of NEt3 and 32.71 g of 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane in 250 ml of anhydrous THF. The mixture is stirred at AT for 30 min. The solvent is evaporated under reduced pressure. Water is added and extraction is carried out with AcOEt. The extract is washed with a 1N aqueous HCl solution, with water and then with a saturated NaCl solution. It is dried over MgSO4 and filtered, and the solvent is evaporated under reduced pressure to give 21 g of the expected product.

Fuente