HRID1055364
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 solution of tert-butyl (2R,3S)-2-methyl-4-oxo-2,3,4,5-tetrahydrobenzo[b][1,4]oxazepin-3-ylcarbamate (0.65 g, 2.22 mmol, Eq: 1.00) in DCM (11.2 mL) at 0° C. was added TFA (12.7 g, 8.26 mL, 111 mmol, Eq: 50.00). After 1 h the mixture was concentrated, the residue dissolved in 50 mL DCM and washed with sat. NaHCO3. The NaHCO3 mixture was extracted with DCM and the combined extracts dried over Na2SO4, filtered and concentrated to afford the title compound (0.42 g, 96%) as a yellow foam which was used without purification.
WORKUP
后处理
- concentrationAfter 1 h the mixture was concentrated
- dissolutionthe residue dissolved in 50 mL DCM
- washwashed with sat. NaHCO3
- extractionThe NaHCO3 mixture was extracted with DCM
- dry with materialthe combined extracts dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated