HRID1925390

反应详情

EQUATION

反应方程式

HRID 1925390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Into a 50 mL round bottom flask was placed 3-bromo-5-(trifluoromethyl)benzenamine (1 g, 4.16 mmol) and DMF (10 mL). To this was added tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate (1.67 g, 5.4 mmol), palladium dichlorodiphenylphosphinoferrocene (183 mg, 0.24 mmol), potassium carbonate (2.29 g, 16.6 mmol). Allowed to heat at 80° C. with stirring for 20 h. Work up: Reaction cooled to RT, solvents removed under reduced pressure. Purified via silica column using 0 to 8% MeOH gradient in DCM. Best fractions pooled, solvents removed under reduced pressure. Affords a clear oil. LC-MS (+) shows mass 343 (N+H) as expected for C17H2lF3N2O2, mw 342.36.

WORKUP

后处理

  1. customInto a 50 mL round bottom flask was placed
  2. customReaction
  3. temperaturecooled to RT
  4. customsolvents removed under reduced pressure
  5. customPurified via silica column
  6. customsolvents removed under reduced pressure
  7. customAffords a clear oil