HRID1747132
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
To a solution of the product of Step A (1.74 g, 3.39 mmol, 1 eq) in methanol (100 mL) at rt under Ar (degassed) was added 0.2 N NaOH (85 mL, 85 mmol, 5 eq) that was degassed by bubbling Ar through the solution prior to addition. After 2 hr, the methanol was concentrated, 6 N HCl was added until the solution was acidic, the aqueous was extracted with DCM, the organics combined, dried over MgSO4 and concentrated to afford the product of Step B which was used unpurified in the next step. Calculated for C22H28F3N3O3S: 494.2 (M+23). found: 494.1.
WORKUP
后处理
- customwas degassed
- customby bubbling Ar through the solution
- additionto addition
- concentrationthe methanol was concentrated
- addition6 N HCl was added until the solution
- extractionthe aqueous was extracted with DCM
- dry with materialdried over MgSO4
- concentrationconcentrated