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
- 100 °C
PROCEDURE
实验过程
A suspension of ethyl 2-(4-bromo-1-(4-chlorophenyl)-3-methylnaphthalen-2-yl)-2-tert-butoxyacetate (25 mg, 51 μmol), trimethylboroxine (21 μL, 0.153 mmol), PdCl2(dppf) (3.7 mg, 5.1 μmol), K2CO3 (70 mg, 0.510 mmol), PhMe (500 μL), EtOH (absolute, 250 μL), and H2O (250 μL) was stirred in a sealed vessel at 100° C. for 3 h. The reaction was cooled to 23° C., diluted with H2O and extracted with EtOAc (3×). Combined organic phases were dried (Na2SO4), filtered, and concentrated, giving crude product. (Yield was not found). 1H NMR (400 MHz, CD3OD) δ 8.08 (d, J=8.2 Hz, 1H), 7.48-7.44 (m, 3H), 7.29-7.26 (m, 4H), 5.15 (s, 1H), 4.20-4.12 (m, 2H), 2.65 (s, 3H), 2.55 (s, 3H), 1.21 (t, J=7 Hz, 3H), 1.00 (s, 9H).
WORKUP
后处理
- temperatureThe reaction was cooled to 23° C.
- extractionextracted with EtOAc (3×)
- dry with materialCombined organic phases were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customgiving crude product
- custom(Yield