HRID470312

反应详情

EQUATION

反应方程式

HRID 470312 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-Chloro-3-[6-(2,8-diaza-spiro[5.5]undec-2-yl)-4-methyl-1H-benzoimidazol-2-yl]-1H-pyridin-2-one (16 mg, 0.039 mmol), (S)-2-amino-1-(3-chlorophenyl)-ethanol (20 mg, 0.117 mmol) and Et3N (16 mg, 0.156 mmol) in EtOH (0.5 mL) was heated at 80° C. for 16 h. After it was cooled to room temperature, the reaction mixture was filtered to furnish yellow solid that was washed with MeOH (3×3 mL). The yellow solid then was mixed with 3 mL MeOH and the mixture was heated at 100° C. for 1 h. After it was cooled to room temperature, the mixture was filtered to furnish yellow solid that was washed with MeOH (3×2 mL) to afford the title compound (10 mg, 47%). ESI-MS m/z 547 (MH+).

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered
  2. customto furnish yellow solid
  3. washthat was washed with MeOH (3×3 mL)
  4. additionThe yellow solid then was mixed with 3 mL MeOH
  5. temperaturethe mixture was heated at 100° C. for 1 h
  6. temperatureAfter it was cooled to room temperature
  7. filtrationthe mixture was filtered
  8. customto furnish yellow solid
  9. washthat was washed with MeOH (3×2 mL)