HRID63634

反应详情

EQUATION

反应方程式

HRID 63634 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a suspension of 5-oxo-5,6,7,8-tetrahydronaphthalen-2-yl 4-methylbenzene-1-sulfonate (1.3 g, 4.4 mmol), 2-methylpyridine-4-boronic acid pinacol ester (800 mg, 3.7 mmol), Na2CO3 (773 mg, 7.3 mmol) and LiCl.H2O (442 mg, 7.3 mmol) in EtOH/H2O/toluene (4.4 mL/2.3 mL/20.0 mL) was added Pd(PPh3)4 (211 mg, 0.2 mmol) at rt under N2. The reaction was stirred at 100° C. overnight. The reaction was filtered and concentrated. Purification by silica gel chromatography (PE:EtOAc=1:1) gave 865 mg (quantitative) of the title compound as a yellow solid. [M+H] Calc'd for C16H15NO, 238. Found, 238.

WORKUP

后处理

  1. filtrationThe reaction was filtered
  2. concentrationconcentrated
  3. customPurification by silica gel chromatography (PE:EtOAc=1:1)