Reaktion #1447129

Reaktionsgleichung

dichloro vinylphosphonate

ethyl-3-hydroxybenzoate

triethylamine

→

desired title compound

Ausbeute 99.5%

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

Ausbeute 99.5%

Lösungsmittel

methylene chloride

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added dropwise at 0° C.
2. 2
   Waschenwashed twice with water (40 mL each)
3. 3
   WaschenThe separated organic layer was washed with brine
4. 4
   Trocknendried over magnesium sulfate
5. 5
   Filtrationfiltered
6. 6
   Sonstigeevaporated to dryness in vacuo

Vorschrift

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]+.

Quelle