HRID13833
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 product of Example 3 (50 mg) in THF (1 mL) was combined with methansulfonyl chloride (15 μL) and triethylamine (27 μL) at 0° C. The reaction stirred 15 minutes at which point methanol (2 mL) was added. The reaction stirred 4.5 hours before it was diluted with EtOAc and washed with water. The organic layer was dried (Na2SO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica eluted with 0-20% EtOAc in hexane afforded the title compound. HPLC/MS: 488.0 (M+1), 490.0 (M+3); Rt=4.45 min.
WORKUP
后处理
- additionwas added
- washwashed with water
- dry with materialThe organic layer was dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification by flash chromatography on silica
- washeluted with 0-20% EtOAc in hexane