HRID1765523

反应详情

EQUATION

反应方程式

HRID 1765523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2-Amino-5-chlorobenzophenone (5.33 g, 23 mmol) was dissolved in 100 mL pyridine and stirred at room temperature. 4-Bromobenzenesulfonyl chloride (6.17 g, 24.1 mmol) was added and the mixture was stirred overnight. The mixture was poured in a steady stream into 350 mL vigorously stirring chilled 6M HCl which resulted in the precipitation of a reddish oil. The solution was diluted with 100 mL EtOAc and 200 mL H2O, shaken in a separating funnel and the aqueous layer discarded. The organics were dried and reduced in vacuo to yield title compound (10.2 g, 98%). 1H NMR (400 MHz, CDCl3): δ 7.34 (m, 5H), 7.43–7.48 (m, 5H), 7.62 (t, 1H), 7.74 (d, 1H), 9.62 (s, 1H). MS: m/z=449.9 (M++1).

WORKUP

后处理

  1. stirringthe mixture was stirred overnight
  2. additionThe mixture was poured in a steady stream into 350 mL
  3. stirringvigorously stirring
  4. customresulted in the precipitation of a reddish oil
  5. stirringshaken in a separating funnel
  6. customThe organics were dried