HRID1747454

反应详情

EQUATION

反应方程式

HRID 1747454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4,6-Dimethyl-1,2-benzisothiazole-3-carboxylic acid (10 mg, 0.048 mmol) in MeOH (5 mL) was added conc. H2SO4 (0.1 mL) at room temperature. The solution was heated up to 60 C for 24 hours. The solution was cooled down and was neutralized with sat. NaHCO3. The solution was extracted with EtOAc. The combined organic layer was dried with MgSO4 and was filtered. The filtrate was concentrated and the residue was purified by CombiFlash with 20% EtOAc in Hexane as the eluent to afford the desirable product 4,6-Dimethyl-benzo[d]isothiazole-3-carboxylic acid methyl ester, CAS: 4,6-Dimethyl-1,2-benzisothiazole-3-carboxylic acid methyl ester (10 mg, 94%) as colorless oil.

WORKUP

后处理

  1. temperatureThe solution was heated up to 60 C for 24 hours
  2. temperatureThe solution was cooled down
  3. extractionThe solution was extracted with EtOAc
  4. dry with materialThe combined organic layer was dried with MgSO4
  5. filtrationwas filtered
  6. concentrationThe filtrate was concentrated
  7. customthe residue was purified by CombiFlash with 20% EtOAc in Hexane as the eluent