Reacción #1447129

Ecuación de reacción

dichloro vinylphosphonate

ethyl-3-hydroxybenzoate

triethylamine

→

desired title compound

Rendimiento 99.5%

Diethyl 3,3′-[(vinylphosphoryl)bis(oxy)]dibenzoate

Rendimiento 99.5%

Disolventes

methylene chloride

methylene chloride

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONwas added dropwise at 0° C.
2. 2
   Lavadowashed twice with water (40 mL each)
3. 3
   LavadoThe separated organic layer was washed with brine
4. 4
   Secadodried over magnesium sulfate
5. 5
   Filtraciónfiltered
6. 6
   Otroevaporated to dryness in vacuo

Procedimiento

A solution containing ethyl-3-hydroxybenzoate (8 mmol, 1.329 g) and triethylamine (8.3 mmol, 829 mg) in methylene chloride (50 mL) was added dropwise at 0° C. under stirring to a solution of dichloro vinylphosphonate (4 mmol, 0.58 g) in methylene chloride (20 mL). The reaction mixture was stirred at ambient temperature for 24 hours, washed twice with water (40 mL each). The separated organic layer was washed with brine, dried over magnesium sulfate, filtered and evaporated to dryness in vacuo to yield 1.61 g (86-99%) of the desired title compound. MS (APPI+): m/e 405 [M+H]+.

Fuente