HRID83630

反应详情

EQUATION

反应方程式

HRID 83630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1-(1-(4-chlorobenzyl)-1H-indole-2-carbonyl)piperidine-4-carboxylic acid (100 mg, 0.252 mmol), EDCI (97 mg, 0.504 mmol), and 1-hydroxybenzotriazole (68.1 mg, 0.504 mmol) were dissolved in DCM (Volume: 3.0 ml). The reaction was stirred at room temperature for 10 minutes before Hunig's Base (0.088 ml, 0.504 mmol) and 2-phenylethanamine (0.063 ml, 0.504 mmol) were added. The reaction was allowed to stir overnight at room temperature. The reaction was diluted with water and ethyl acetate. The organic phase was washed with 1N HCl, saturated sodium bicarbonate, and brine. The organic phase was dried over magnesium sulfate, filtered, and concentrated. The crude material was recrystallized in ether and ethyl acetate to obtain product as a white solid. (Yield: 76 mg, white solid) 1H-NMR (400 MHz, DMSO-d6) 7.85, 7.62, 7.53, 7.36-7.05, 6.71, 5.48, 4.38, 4.01, 3.26, 2.90, 2.69, 2.39-2.28, 1.61, 1.36

WORKUP

后处理

  1. additionwere added
  2. washThe organic phase was washed with 1N HCl, saturated sodium bicarbonate, and brine
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude material was recrystallized in ether
  7. customethyl acetate to obtain product as a white solid