反応 #2195497

反応方程式

diethyl 3-oxopentanedioate

sodium bicarbonate

Lawesson's reagent

→

title compound

Diethyl 3-thioxopentanedioate

溶媒

toluene

反応条件

後処理

1. 1
   温度then heat
2. 2
   温度under reflux for 5 h
3. 3
   温度Cool
4. 4
   ろ過filter
5. 5
   濃縮concentrate in vacuo
6. 6
   その他Purify the residue by silica gel chromatography

実験手順

Dissolve 14.1 mmol of diethyl 3-oxopentanedioate in 15 mL of toluene under argon add 49.4 mmol of sodium bicarbonate and 15.1 mmol of Lawesson's reagent. Stir for 1 h at room temperature then heat under reflux for 5 h. Cool, filter, and concentrate in vacuo. Purify the residue by silica gel chromatography using ethyl acetate/hexanes eluant to yield the title compound.

出典