HRID1976419

反应详情

EQUATION

反应方程式

HRID 1976419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of methyl1-[{[4-(2- butynyloxy)phenyl]sulfonyl}(methyl)amino]cyclohexanecarboxylate (4.6 g, 12.1 mmol) in methanol:THF (4:1, 100 ml), 10 N sodium hydroxide (15 ml) was added at room temperature. The reaction was stirred for 16 h and evaporated to dryness in vacuo and the residue was dissolved in 100 mL water. The pH was adjusted to 1 with 5N hydrochloric acid solution and the mixture was extracted with chloroform, washed with water, dried and concentrated to give 1-[{[4-(2-butynyloxy)phenyl]sulfonyl}(methyl)amino] cyclohexanecarboxylic acid as a yellow solid. Yield: 4 g(88%); mp 124-6° C. Electrospray Mass Spec 364(M−H)−.

WORKUP

后处理

  1. customevaporated to dryness in vacuo
  2. dissolutionthe residue was dissolved in 100 mL water
  3. extractionthe mixture was extracted with chloroform
  4. washwashed with water
  5. customdried
  6. concentrationconcentrated