HRID1628148

反应详情

EQUATION

反应方程式

HRID 1628148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-Hydroxy-benzoic acid methyl ester (3.19 g, 21 mmol) was dissolved together with pyridine (1.97 g, 25 mmol) in dry THF (20 mL) and after cooling down to 0° C., methanesulfonyl chloride (2.29 g, 20 mmol) was added dropwise. The ice bath was removed and mixture was stirred at r.t. for 5 h. After diluting with DCM and extraction with water and aq. HCl (2N), the organic layer was dried (MgSO4) and evaporated to afford the crude but highly pure product as a solid which was used in the next step without further purification (4.38 g, 95.1%). 1H NMR (400 MHz, CDCl3): δ 8.07-8.09 (d, 2H), 7.32-7.34 (d, 2H), 3.90 (s, 3H), 3.16 (s, 3H).

WORKUP

后处理

  1. customThe ice bath was removed
  2. additionAfter diluting with DCM and extraction with water and aq. HCl (2N)
  3. dry with materialthe organic layer was dried (MgSO4)
  4. customevaporated
  5. customto afford the crude but highly pure product as a solid which
  6. customwas used in the next step without further purification (4.38 g, 95.1%)