반응 #1447129

반응 방정식

dichloro vinylphosphonate

ethyl-3-hydroxybenzoate

triethylamine

→

desired title compound

수율 99.5%

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

수율 99.5%

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise at 0° C.
2. 2
   세척washed twice with water (40 mL each)
3. 3
   세척The separated organic layer was washed with brine
4. 4
   건조dried over magnesium sulfate
5. 5
   여과filtered
6. 6
   기타evaporated to dryness in vacuo

실험 절차

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]+.

출처