HRID2079083

反应详情

EQUATION

反应方程式

HRID 2079083 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a reaction vial charged with 8-fluoro-4H-thieno[3,2-c]chromene-2-carbonyl chloride (0.120 g, 0.447 mmol) and 2,4-difluoroaniline (0.0959 g, 0.670 mmol) was added a catalytic amount of DMAP. Pyridine in methylene chloride (1.2 M, 1.49 mL) was added. The reaction was stirred at room temperature with LC/MS monitor. The reaction was complete in a couple hours. After aqueous work up, the reaction was concentrated in vacuo, taken into DMF at a concentrated of 100 mg/ml and purified by preparative RP-HPLC to give 163bp. Yield=31% of theoretical. MS: (ESI+)=376.4

WORKUP

后处理

  1. customTo a reaction
  2. concentrationAfter aqueous work up, the reaction was concentrated in vacuo
  3. concentrationa concentrated of 100 mg/ml
  4. custompurified by preparative RP-HPLC
  5. customto give 163bp