HRID1820885

反应详情

EQUATION

反应方程式

HRID 1820885 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(3,4-Dimethoxy-phenyl)-1H-pyrrolo-[2,3-b]pyridine 1 (50 mg, 0.20 mmol) was dissolved in N,N-dimethylformamide (4 mL). Sodium hydride (10 mg, 0.24 mmol, 60% dispersion in mineral oil) was added. The reaction mixture was stirred for 15 minutes at room temperature. 1-Isothiocyanatobenzene (35 μL, 0.29 mmol) was added and the reaction mixture was stirred for 40 minutes at room temperature. The product was concentrated and the residue was partitioned between brine and ethyl acetate. The organic portion was dried over anhydrous sodium sulfate, filtered, and concentrated to provide a solid. The solid was washed with a minimum of methanol and dried in vacuo to provide 41, (38 mg, 49%). MS(ESI) [M+H+]+=390.2.

WORKUP

后处理

  1. stirringthe reaction mixture was stirred for 40 minutes at room temperature
  2. concentrationThe product was concentrated
  3. customthe residue was partitioned between brine and ethyl acetate
  4. dry with materialThe organic portion was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto provide a solid
  8. washThe solid was washed with a minimum of methanol
  9. customdried in vacuo