HRID2175900

反应详情

EQUATION

反应方程式

HRID 2175900 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a flask charged with methyl 2-amino-6,7-dihydro-5H-cyclopenta[b]pyridine-5-carboxylate (500 mg, 2.6 mmol) and a stir bar was added sodium azide (340 mg, 5.2 mmol), triethyl orthoformate (2.2 mL, 13 mmol), and HOAc (10 mL). The mixture was heated to 100° C. for 2 hours. The solvent was removed on a rotavapor, and the residue was taken into aq. sodium carbonate, extracted with EtOAc (50 mL×3), dried over sodium sulfate, and purified by MPLC (DCM-MeOH). After removal of solvent, the title compound was collected. LC-MS (IE, m/z): 248 [M+1]+.

WORKUP

后处理

  1. customThe solvent was removed on a rotavapor
  2. extractionextracted with EtOAc (50 mL×3)
  3. dry with materialdried over sodium sulfate
  4. custompurified by MPLC (DCM-MeOH)
  5. customAfter removal of solvent
  6. customthe title compound was collected