HRID23462

反应详情

EQUATION

反应方程式

HRID 23462 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 4-isopropyl-7-methyl-6-thiocyanato-benzothiazol-2-yl-amine (Example L-4; 4.0 g, 17 mmol) dissolved in CH2Cl2 (25 mL) and pyridine (5 mL), was added methyl chloroformate at 0° C. The reaction mixture was stirred at room temperature for 2 hours. H2O was added to the reaction mixture followed by EtOAc (100 mL). The organic layer was washed with 2N HCl, H2O, saturated sodium bicarbonate solution and brine, and was dried (MgSO4). The solvents were evaporated, and the residue was purified by flash chromatography (100% hexanes to 25% EtOAc in hexanes) to give 2-(methyloxycarbonyl)amino-4-isopropyl-7-methyl-6-thiocyanato-benzothiazole. MS (APCI): 322 (M+H).

WORKUP

后处理

  1. washThe organic layer was washed with 2N HCl, H2O, saturated sodium bicarbonate solution and brine
  2. dry with materialwas dried (MgSO4)
  3. customThe solvents were evaporated
  4. customthe residue was purified by flash chromatography (100% hexanes to 25% EtOAc in hexanes)