HRID1466043

反应详情

EQUATION

反应方程式

HRID 1466043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of tert-Butyl (2-{(chloroacetyl)[(5-cyano-2,3-dihydro-1H-inden-2-yl)methyl]amino}ethyl)carbamate (350 mg, 0.9 mmol) in HCl/dioxane (20 mL) was stirred at RT for 12 hours and then concentrated to dryness. To the residue was added 20 mL EtOH and K2CO3 (500 mg, 3.7 mmol). The resulting mixture was heated to reflux for 4 hrs before cooled to RT and filtered. The filtrate was concentrate and the residue was partitioned between EtOAc and water. The organic layer was washed with brine, dried over anhydrous Na2SO4 and concentrated to dryness to give 2-[(2-Oxopiperazin-1-yl)methyl]indane-5-carbonitrile. MS m/z: 256 [M+1]+.

WORKUP

后处理

  1. concentrationconcentrated to dryness
  2. temperatureThe resulting mixture was heated
  3. temperatureto reflux for 4 hrs
  4. temperaturebefore cooled to RT
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrate
  7. customthe residue was partitioned between EtOAc and water
  8. washThe organic layer was washed with brine
  9. dry with materialdried over anhydrous Na2SO4
  10. concentrationconcentrated to dryness