HRID1435356
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 stirred suspension of the protected amine (940 mg, 2.16 mmol, Example 319) in methylene chloride (30 mL), trifluoroacetic acid (20 mL) was added at 0° C. and the mixture stirred for 2 hours. The solvent was removed and the residue was partitioned between ethyl acetate and 5% sodium carbonate solution. The aqueous layer was extracted with ethyl acetate/tetrahydrofuran (1:1, 3×10 ml). The extracts were combined and the solution was dried with sodium sulfate. Removal of solvent gave a yellow solid. 711 mg, 98%. MS (ES) MH+=336.
WORKUP
后处理
- additionwas added at 0° C.
- customThe solvent was removed
- customthe residue was partitioned between ethyl acetate and 5% sodium carbonate solution
- extractionThe aqueous layer was extracted with ethyl acetate/tetrahydrofuran (1:1, 3×10 ml)
- dry with materialthe solution was dried with sodium sulfate
- customRemoval of solvent
- customgave a yellow solid