HRID595357

反应详情

EQUATION

反应方程式

HRID 595357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

This reaction is carried out in the same manner as the reaction in example 3. The difference is that, the reactants are p-methoxyphenyl chloride (142.2 mg, 1.0 mmol), acetophenone (302.1 mg, 2.5 mmol), palladium cinnamyl chloride (7.8 mg, 0.015 mmol), 2-Methoxy-6-(N-methyl-N-phenyl-amino)phenyldicyclohexyl)phosphine (18.4 mg, 0.045 mmol), K3PO43H2O (664.0 mg, 2.5 mmol) in 3 mL dry toluene at 110° C. for 16.7 h. 2-(4′-Methoxyphenyl)-1-phenyl-1-ethanone (177.3 mg) was obtained with a yield of 79% as solid. m.p.: 94.1-94.4° C. (n-hexane); 1H NMR (300 MHz, CDCl3) δ 8.07-8.00 (m, 2H, ArH), 7.60-7.51 (m, 1H, ArH), 7.51-7.42 (m, 2H, ArH), 7.25-7.17 (m, 2H, ArH), 6.92-6.86 (m, 2H, ArH), 4.24 (s, 2H, CH2), 3.78 (s, 3H, OCH3); 13C NMR (75 MHz, CDCl3) δ 197.8, 158.3, 136.4, 132.9, 130.3, 128.45, 128.41, 126.3, 113.9, 55.0, 44.4; IR (KBr) v (cm−1) 3056, 2998, 2954, 2934, 2905, 2835, 1691, 1612, 1596, 1579, 1514, 1463, 1447, 1411, 1335, 1301, 1245, 1218, 1204, 1178, 1107, 1035; MS (70 eV, EI) m/z (%): 227 (M++1, 3.58), 226 (M+, 21.25), 121 (100).

WORKUP

后处理

  1. customThis reaction is carried out in the same manner as the reaction in example 3
  2. customat 110° C.
  3. customfor 16.7 h