HRID711268

反应详情

EQUATION

反应方程式

HRID 711268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a reaction vial was added (6-chloro-5-methylpyridin-3-yl)methanamine 30-4 (500 mg, 2.6 mmol), 2-methylpyridin-4-ylboronic acid 15-1 (460 mg, 3.38 mmol), Pd(OAc)2 (58 mg, 0.26 mmol), S-Phos (150 mg, 0.37 mmol) and K3PO4 (1.65 g, 7.8 mmol). The vial was evacuated and backfilled with nitrogen. 2-butanol (5 mL) was added via syringe. The reaction was stirred at room temperature for 10 mins and then 110° C. for 2 hours. After cooling to room temperature, the reaction mixture was diluted into 10% methanol in DCM, and filtered through celite pad. The filtrate was dried and the crude product was purified by silica gel flash chromatography, and eluted with 10% methanol in DCM to give (2′,3-dimethyl-2,4′-bipyridin-5-yl)methanamine 63-2 as an oil. MS m/z 214.2 (M+1).

WORKUP

后处理

  1. customThe vial was evacuated
  2. addition2-butanol (5 mL) was added via syringe
  3. wait110° C. for 2 hours
  4. temperatureAfter cooling to room temperature
  5. additionthe reaction mixture was diluted into 10% methanol in DCM
  6. filtrationfiltered through celite pad
  7. customThe filtrate was dried
  8. customthe crude product was purified by silica gel flash chromatography
  9. washeluted with 10% methanol in DCM