HRID841143
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 from Step 2 (1.8 g, 2.4 mmol) was dissolved in tetrahydrofuran (10 mL), methanol (10 mL) and water (2 mL). Sodium hydroxide (0.192 g, 4.8 mmol) was added and the mixture stirred overnight at room temperature. The solution was concentrated in vacuo and the residue taken up in 0.1 M NaPO4 buffer (100 mL). The pH was brought to 6 by the addition of 1N HCl. The product was extracted three times with ethyl acetate. The ethyl acetate was washed twice with brine, dried over MgSO4, filtered and concentrated in vacuo to give a white powder; 1.3 g (74% yield). MS-APCI: M+1=732.
WORKUP
后处理
- concentrationThe solution was concentrated in vacuo
- additionThe pH was brought to 6 by the addition of 1N HCl
- extractionThe product was extracted three times with ethyl acetate
- washThe ethyl acetate was washed twice with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give a white powder