HRID361388
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 compound from step 164c (4.3 g, 15.6 mmol) was dissolved in 30 mL of 4N HCl in ethanol, and the reaction mixture was stirred for 1.5 hours at room temperature. The solvent was stripped and chased with ether. The residue was dissolved in water, NaCl was added, and the mixture was extracted with ethyl ether, which was discarded. The aqueous layer was adjusted to pH 12 with K2CO3, saturated with NaCl, then extracted with CHCl3. The organic extract was washed with brine, dried (Na2SO4) and filtered. The solvent was removed under vacuum to afford 2.17 g of the title compound. MS m/z (M+H)+ : 177, MS m/z (M+NH4)+ : 194.
WORKUP
后处理
- extractionthe mixture was extracted with ethyl ether, which
- extractionextracted with CHCl3
- extractionThe organic extract
- washwas washed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customThe solvent was removed under vacuum