反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
The intermediate from Step 2 (280 mg, 0.7 mmol) was combined with benzyl 2,4-bis(benzyloxy)-6-chloro-5-methylnicotinate (332 mg, 0.7 mmol, prepared according to Example 379, Step 3), potassium carbonate (193 mg, 1.4 mmol), tris(dibenzylideneacetone) dipalladium(0) (32 mg, 0.035 mmol) and tri-tert-butylphosphine tetrafluoroborate (41 mg, 0.14 mmol) in DMSO (3 mL). The mixture was heated under Ar at 120° C. for 20 min. The mixture was cooled to room temperature and partitioned in CH2Cl2 (10 mL) and saturated aqueous NaHCO3 (10 mL). The organic layer was removed, concentrated and chromatographed on silica gel (0-30% EtOAc in hexanes) to provide the product as a white powder (274 mg, 55%).
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- custompartitioned in CH2Cl2 (10 mL)
- customThe organic layer was removed
- concentrationconcentrated
- customchromatographed on silica gel (0-30% EtOAc in hexanes)