HRID1047686
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The mixture of 4-(2-isopropoxy-3-methyl-benzoylamino)-tetrahydro-thiopyran-4-carboxylic acid methyl ester (28) (75 mg, 0.21 mmol) and KOH (500 mg, 8.9 mmol) is dissolved in EtOH (5 mL) and water (0.5 mL) under a water bath. The water bath is removed when KOH is completely dissolved and the resulting reaction solution is stirred at RT for 8 h. After concentration in vacuo, the residue is dissolved in water (20 mL) and acidified with conc. HCl until no more precipitate came out of the water. The precipitate is filtered to give a pure product (29) as a pale yellow solid (68 mg, 94%).
WORKUP
后处理
- customThe water bath is removed when KOH
- dissolutionis completely dissolved
- customthe resulting reaction solution
- concentrationAfter concentration in vacuo
- dissolutionthe residue is dissolved in water (20 mL)
- filtrationThe precipitate is filtered