HRID2174243
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
Compound 83 (15 mg, 0.044 mmol) was dissolved in dry THF (0.8 mL) and this solution added to the phenyl magnesium bromide (1M, 0.2 mL, 0.20 mmol) at 0° C. The mixture was stirred and allowed to warm slowly to RT. The mixture was quenched with MeOH/HCl (2M) (1 mL:0.1 mL) then NH4Cl (sat.) added and the mixture diluted with water and EtOAc (pH of aqueous ˜7). The mixture was extracted into EtOAc and the organics combined and dried with brine then Na2SO4. The solvent was removed to afford 20 mg crude residue. This was dissolved in DCM (2 mL) and applied to a silica column, eluting with EtOAc/heptane, to afford Compound 112 (13 mg).).
WORKUP
后处理
- customThe mixture was quenched with MeOH/HCl (2M) (1 mL:0.1 mL)
- additionNH4Cl (sat.) added
- additionthe mixture diluted with water and EtOAc (pH of aqueous ˜7)
- extractionThe mixture was extracted into EtOAc
- dry with materialdried with brine
- customThe solvent was removed
- customto afford 20 mg crude residue
- washeluting with EtOAc/heptane