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
A solution of methanolic hydrogen chloride (approx. 1.6M, 1.5 mL) was added to 6-[(3R)-3-(tert-butoxycarbonylamino)-4-(2,4,5-trifluorophenyl)butanoyl]-5-ethyl-5,6,7,8-tetrahydropyrido[3,4-b]pyrazine (18 mg, 0.038 mmol) dissolved in 0.25 mL of methanol. After 2.5 h, the solution was added to saturated aqueous sodium bicarbonate solution (10 mL), which was then extracted with two portions of ethyl acetate (25 mL and 15 mL). The organic layers were washed in succession with saturated aqueous brine (5 mL), dried over sodium sulfate, decanted, and concentrated. The residue was dissolved in methanol, and the resulting solution was filtered (0.45 micron PTFE membrane) and evaporated to provide the title compound as a very viscous colorless syrup. LC/MS: 379 (M+1).
WORKUP
后处理
- extractionwas then extracted with two portions of ethyl acetate (25 mL and 15 mL)
- washThe organic layers were washed in succession with saturated aqueous brine (5 mL)
- dry with materialdried over sodium sulfate
- customdecanted
- concentrationconcentrated
- dissolutionThe residue was dissolved in methanol
- filtrationthe resulting solution was filtered (0.45 micron PTFE membrane)
- customevaporated