HRID1466076

反应详情

EQUATION

反应方程式

HRID 1466076 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of tert-Butyl [(4-cyano-5-fluoro-2,3-dihydro-1H-inden-1-yl)methyl]prop-2-en-1-ylcarbamate (45 mg, 0.14 mmol) in MeOH (5 mL) was bubbled ozone until the solution turned blue. Excess ozone was removed by bubbling nitrogen through. To the reaction was then added DMS (0.50 ml, 6.8 mmol), and it was allowed to warm to RT. The solvent was removed under reduced pressure, and the resulting material was further treated with ethyl aminoacetate hydrochloride (13 mg, 0.090 mmol) and sodium cyanoborohydride (6.0 mg, 0.090 mmol). When LC showed the reaction was done, the reaction was diluted with EtOAc, washed with brine, dried over sodium sulfate, and purified by MPLC to deliver the title product. LC-MS (IE, m/z): 420 [M+1]+.

WORKUP

后处理

  1. customExcess ozone was removed
  2. customby bubbling nitrogen through
  3. customThe solvent was removed under reduced pressure
  4. washwashed with brine
  5. dry with materialdried over sodium sulfate
  6. custompurified by MPLC