HRID427399
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 2-tert-butoxycarbonylamino-N-methoxy-N-methyl succinamic acid benzyl ester (0.50 g, 1.36 mmol) in THF (5 mL) at −78° C. was added DIBAL-H (0.233 g, 1.67 mmol) dropwise. The mixture was stirred for 1.5 h and monitored by TLC. When completed the reaction was quenched with 5 mL of saturated solution of Rochell salt (KNaC4H4O6.4H2O) (potassium sodium tartrate) and extracted with EtOAc (2×10 mL). The organic layer was washed with H2O, brine, dried over Na2SO4, filtered and concentrated in vacuo to give the title compound in quantitative yield (0.40 g).
WORKUP
后处理
- customwas quenched with 5 mL of saturated solution of Rochell salt (KNaC4H4O6.4H2O) (potassium sodium tartrate)
- extractionextracted with EtOAc (2×10 mL)
- washThe organic layer was washed with H2O, brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo