Реакция #2195497
ord-785bf6da1b014f6d91aa47772a600156
Уравнение реакции
diethyl 3-oxopentanedioate
sodium bicarbonate
Lawesson's reagent
→
title compound
Diethyl 3-thioxopentanedioate
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураthen heat
- 2Температураunder reflux for 5 h
- 3ТемператураCool
- 4Фильтрацияfilter
- 5Концентрированиеconcentrate in vacuo
- 6ДругоеPurify the residue by silica gel chromatography
Методика
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.