HRID1642136

反应详情

EQUATION

反应方程式

HRID 1642136 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

Methyl 1-(4-methoxyphenylsulfonamido)cyclohexanecarboxylate (27 g, 82.5 mmol) was dissolved in acetone (450 ml), and K2CO3 (22.8 g, 165 mmol) was added thereto. Methyl iodide (10.3 ml, 165 mmol) was then added, and the suspension was heated overnight at 40° C. in a closed flask. Because the reaction was not yet complete (TLC monitoring, heptane/ethyl acetate 2:1), methyl iodide (7.7 ml, 124 mmol) was again added and stirring was carried out over the weekend at room temperature. Methyl iodide (2.6 ml, 41.8 mmol) was again added, and stirring was carried out overnight at 40° C. After cooling, the solid materials were filtered off and the filtrate was concentrated to dryness. The crude product was used further without being purified further.

WORKUP

后处理

  1. additionwas again added
  2. customwas carried out over the weekend at room temperature
  3. stirringstirring
  4. temperatureAfter cooling
  5. filtrationthe solid materials were filtered off
  6. concentrationthe filtrate was concentrated to dryness
  7. customwithout being purified further