HRID1795981

反应详情

EQUATION

反应方程式

HRID 1795981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(±)-(3-{[(3-Benzyl-5-chloro-4-oxo-3,4-dihydro-pyrrolo[2,1-f][1,2,4]triazin-2-yl)-cyclopropyl-methyl]-amino}-propyl)-carbamic acid tert-butyl ester (Example 22H, 16 mg, 0.033 mmol) in methylene chloride (1.5 mL) was treated with triethylamine (5 μL, 0.036 mmol), and p-chlorobenzoyl chloride (6 mg, 0.034 mmol) at 0° C. and the resulting mixture was stirred at room temperature for 1 h. The mixture was diluted with methylene chloride (5 mL), washed with saturated sodium bicarbonate, dried (MgSO4) and concentrated. The residue was purified by flash column chromatography on silica gel eluting with ethyl acetate/hexanes to give the title compound (8 mg) as a clear oil: MS (ESI+) 604.2 (M++H).

WORKUP

后处理

  1. washwashed with saturated sodium bicarbonate
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customThe residue was purified by flash column chromatography on silica gel eluting with ethyl acetate/hexanes