HRID2204540

反应详情

EQUATION

反应方程式

HRID 2204540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Aqueous NaOH (2N, 0.3 mL) was added to 8-cyclohexyl-3-tosyl-3H-imidazo[1,2-a]pyrrolo[2,3-e]pyrazine (0.051 g, 0.13 mmol) in 1,4-dioxane (3 mL) and the mixture was heated at reflux for about 1 h. The organic solvent was removed under reduced pressure and the aqueous phase neutralized with aqueous 1 N HCl and extracted with EtOAc (2×15 mL). The combined organic extracts were washed with brine (1×10 mL), dried over anhydrous MgSO4, and concentrated in vacuo. The residue was suspended in MeCN (2 mL) and the precipitate was collected by filtration and dried to yield 8-cyclohexyl-3H-imidazo[1,2-a]pyrrolo[2,3-e]pyrazine as a tan solid (0.006 g, 19%): LC/MS (Table 2, Method a) Rt=2.12 min; MS m/z: 241 (M+H)+.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for about 1 h
  3. customThe organic solvent was removed under reduced pressure
  4. extractionextracted with EtOAc (2×15 mL)
  5. washThe combined organic extracts were washed with brine (1×10 mL)
  6. dry with materialdried over anhydrous MgSO4
  7. concentrationconcentrated in vacuo
  8. filtrationthe precipitate was collected by filtration
  9. customdried