Реакция #599764
ord-2660a104f465464fa90006c262d38d39
Уравнение реакции
Lead tetraacetate
4-benzyloxy-2,6-dimethylphenyl boronic acid
potassium carbonate
→
4-benzyloxy-2,6-dimethylphenyl lead triacetate
Реагенты
Условия реакции
Температура
50°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Другоеthoroughly flushed with nitrogen
- 2workup.ADDITIONChloroform (20 ml) is added
- 3ТемператураAfter further heating at 50° C. for 3 hours the reaction mixture
- 4Температураis cooled to 0° C.
- 5Фильтрацияbefore filtering
- 6Другоеevaporation of the crude solution under reduced pressure
- 7ДругоеThe crude product is then azeotroped with diethyl ether
Методика
Lead tetraacetate (5.7 g, 0.013 mol) and mercury (II) acetate (0.2 g, 0.0006 mol) are stirred together and thoroughly flushed with nitrogen. Chloroform (20 ml) is added and the dark orange solution heated to 50° C., followed by the addition of 4-benzyloxy-2,6-dimethylphenyl boronic acid (3 g, 0.012 mol) in one portion. After further heating at 50° C. for 3 hours the reaction mixture is cooled to 0° C. and potassium carbonate added (1.9 g, 0.02 mol). The suspension is stirred for just 5 minutes before filtering and evaporation of the crude solution under reduced pressure. The crude product is then azeotroped with diethyl ether to afford 4-benzyloxy-2,6-dimethylphenyl lead triacetate as a pale solid.