HRID1487073

反应详情

EQUATION

反应方程式

HRID 1487073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a stirred solution of methyl 5-(chlorosulfonyl)-2-methoxybenzoate (1 g, 3.78 mmol) in pyridine (3 mL) at 25° C. was added N-isobutyl-2,4-dimethylaniline (0.670 g, 3.78 mmol) and the reaction mixture stirred at 25° C. for 2 hours, then stood for 12 hours. The pyridine was evaporated in vacuo to give a yellow oil which was purified by silica (Si) chromatography (0-50% ethyl acetate-cyclohexane). The appropriate fractions were combined and evaporated in vacuo to give the required product, 1.485 g, as a colourless oil. LCMS [LCMS2] Rt 1.37 min, m/z (ES+) 406 (M+H).

WORKUP

后处理

  1. waitstood for 12 hours
  2. customThe pyridine was evaporated in vacuo
  3. customto give a yellow oil which
  4. customwas purified by silica (Si) chromatography (0-50% ethyl acetate-cyclohexane)
  5. customevaporated in vacuo