HRID1055364

反应详情

EQUATION

反应方程式

HRID 1055364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationAfter 1 h the mixture was concentrated
  2. dissolutionthe residue dissolved in 50 mL DCM
  3. washwashed with sat. NaHCO3
  4. extractionThe NaHCO3 mixture was extracted with DCM
  5. dry with materialthe combined extracts dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated