反应详情

温度

-100 °C

Under argon, an n-butyllithium solution in hexane (1.55N, 6.6 ml) is added dropwise to a solution of 3,5-dibromo-4-methylpyridine (intermediate 10.1, 2.51 g, 10 mmol) kept at −100° C. After stirring for 10 min, tert-butyl isocyanate (2.28 ml, 20 mmol) is added. The stirring is maintained for 20 min at −100° C. and then for 1 h at −78° C. and at room temperature overnight. An aqueous NH4Cl solution is added to the reaction mixture. Extraction with AcOEt/H2O gives a brown solid which is taken up in an AcOEt/petroleum ether mixture. The compound obtained is isolated by filtration.

1. customkept at −100° C
2. waitfor 1 h at −78° C.
3. customat room temperature
4. customovernight
5. extractionExtraction with AcOEt/H2O
6. customgives a brown solid which
7. customThe compound obtained
8. customis isolated by filtration