HRID2099702
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 mixture of 21 mg (0.06 mmol) of 1D in 0.5 mL of THF, 0.5 mL of methanol, and 1 mL of water was added 50 mg (1.19 mmol) of lithium hydroxide monohydrate as solid. The reaction mixture was allowed to stir at room temperature for 2.5 hours and concentrated to dryness. To the residue, 10 mL of water was added, and pH of the resulting mixture was adjusted to 2 using phosphoric acid. This was extracted with 3×35 mL of ethyl acetate. Organic layers were combined, dried (anhydrous Na2SO4) and concentrated to dryness to give 10 mg (0.029 mmol, 53%) of 1M (M+Na, 360).
WORKUP
后处理
- concentrationconcentrated to dryness
- additionTo the residue, 10 mL of water was added
- extractionThis was extracted with 3×35 mL of ethyl acetate
- dry with materialdried (anhydrous Na2SO4)
- concentrationconcentrated to dryness
- customto give 10 mg (0.029 mmol, 53%) of 1M (M+Na, 360)