Реакция #1771211

Уравнение реакции

Lithium aluminum hydride

diethyl ether

4-(3,5-dimethoxy-4-hydroxyphenyl)-1,3-dithiolane-2-thione

→

1-(3,5-dimethoxy-4-hydroxyphenyl)-1,2-ethanedithiol

Растворители

THF

THF

Условия реакции

Обработка

1. 1
   Другое(1 hour)
2. 2
   Другоеthe excess hydride destroyed with H2O
3. 3
   Экстракцияimmediately extracted with diethyl ether
4. 4
   ПромывкаThe organic layer was washed with H2O
5. 5
   Сушкаdried over MgSO4
6. 6
   Фильтрацияfiltered
7. 7
   Другоеevaporated to a white solid (1.64 g, 96%)

Методика

Lithium aluminum hydride (0.553 g, 14.58 mmole) is added to 10 ml dry diethyl ether and 10 ml dry THF. To this slurry is added dropwise 4-(3,5-dimethoxy-4-hydroxyphenyl)-1,3-dithiolane-2-thione (34) (2.00 g, 6.94 mmole) predissolved in 40 ml dry THF. The reaction is stirred under a nitrogen (N2) atmosphere until the solution becomes colorless (1 hour). The reaction is cooled to 0° C. and the excess hydride destroyed with H2O. The reaction mixture is acidified with 10% HCl and immediately extracted with diethyl ether. The organic layer was washed with H2O, dried over MgSO4, filtered and evaporated to a white solid (1.64 g, 96%).

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