HRID1175571

反应详情

EQUATION

反应方程式

HRID 1175571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

2-(4-Bromophenyl)-N-isobutyl-2-methylpropanamide (Example 1a) (100 mg, 0.33 mmol) was weigh out in a microwave vial and dissolved in 3 ml of DME, 2 ml of EtOH and 1.5 ml of water followed by addition of Na2CO3 (70 mg, 0.66 mmol) and 3-nitrophenylboronic acid (67 mg, 0.4 mmol). Pd(PPh3)4 (8 mg, 6.6 μmol) was then added and the tube was immediately sealed. The reaction mixture was heated in a Smith Synthesizer at 150° C. for 5 min. The solution was filtered and the compound purified by preparative HPLC to yield 75 mg (67%) of the title compound as a white solid. 1H NMR (400 MHz, CDCl3): δ 0.8 (d, 6H), 1.65 (s, 6H), 1.67-1.70 (m,1H), 3 (dd, 2H), 5.2 (broad, 1H), 7.5(d, 2H), 7.6 (d, 3H), 7.9 (d, 1H), 8.2 (dd, 1H), 8.4 (d, 1H). MS (M+H, 341).

WORKUP

后处理

  1. customthe tube was immediately sealed
  2. filtrationThe solution was filtered
  3. customthe compound purified by preparative HPLC