反応 #1447129

反応方程式

dichloro vinylphosphonate

ethyl-3-hydroxybenzoate

triethylamine

→

desired title compound

収率 99.5%

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

収率 99.5%

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   workup.ADDITIONwas added dropwise at 0° C.
2. 2
   洗浄washed twice with water (40 mL each)
3. 3
   洗浄The separated organic layer was washed with brine
4. 4
   乾燥dried over magnesium sulfate
5. 5
   ろ過filtered
6. 6
   その他evaporated to dryness in vacuo

実験手順

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]+.

出典