反応 #422249

反応方程式

methyl 2-(bis(2,4,6-trimethylbenzoyl)-phosphinyl)acetate

2-propyn-1-ol

dibutyltin dilaurate

→

propyn-3-yl 2-[bis(2,4,6-trimethylbenzoyl)-phosphoryl]acetate

収率 55.0%

反応条件

後処理

1. 1
   workup.DISTILLATIONExcess 2-propyn-1-ol is distilled off under vacuum
2. 2
   その他the residual oil purified by preparative column chromatography (silica gel, eluent toluene/ethyl acetate 9:1)

実験手順

2.9 g (7 mmol) methyl 2-(bis(2,4,6-trimethylbenzoyl)-phosphinyl)acetate (example 22) is dissolved in a tenfold excess of 2-propyn-1-ol and heated to 90° C. during 12 hours in the presence of 10 mol % dibutyltin dilaurate. Excess 2-propyn-1-ol is distilled off under vacuum and the residual oil purified by preparative column chromatography (silica gel, eluent toluene/ethyl acetate 9:1). 1.7 g (55%) propyn-3-yl 2-[bis(2,4,6-trimethylbenzoyl)-phosphoryl]acetate are obtained as yellowish oil.

出典