HRID1859801

反应详情

EQUATION

反应方程式

HRID 1859801 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The product obtained from Step 2 (0.180 g, 0.68 mmol) was dissolved in 5 mL of dry DMF and treated with K2CO3 (0.376 g, 2.72 mmol) and 4-(2-bromoethyl)imidazole hydrobromide (0.192 g, 0.75 mmol). After stirring overnight at room temperature, the reaction was diluted with water and extracted with EtOAc. The pooled extracts were washed well with aqueous 0.5N KOH, water and brine, and then dried, filtered, and concentrated. Purification of the residue (SiO2, 5% MeOH in DCM) afforded 0.120 g (49%) of the title compound as a light yellow foam. Conversion of this product to its HCl salt according to the method of Example 34 afforded 0.063 g of a light yellow powder, mp 170-172° C.: CI-MS m/e 359 (M++1).

WORKUP

后处理

  1. extractionextracted with EtOAc
  2. washThe pooled extracts were washed well with aqueous 0.5N KOH, water and brine
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification of the residue (SiO2, 5% MeOH in DCM)