HRID20603

反应详情

EQUATION

反应方程式

HRID 20603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-[4-(azetidin-1-ylcarbonyl)-2-chlorophenoxy]-5-((1S)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-methylethoxy)-N-pyrazin-2-ylbenzamide (37 mg, 0.062 mmol) in methanol (0.5 mL) and 3.5M hydrochloric acid (0.018 mL) was stirred for 30 mins at RT. The solution was taken to pH 6 with saturated aqueous sodium bicarbonate solution and the volatiles were removed in vacuo. The residue was taken into ethyl acetate (10 mL) and washed with water (2 mL), brine (2 mL), dried (MgSO4), filtered and the solvents removed in vacuo to give the crude product which was chromatographed on silica, eluting with 0-10% methanol in ethyl acetate, to give the desired compound as a white foam (21 mg).

WORKUP

后处理

  1. customthe volatiles were removed in vacuo
  2. washwashed with water (2 mL), brine (2 mL)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvents removed in vacuo
  6. customto give the crude product which
  7. customwas chromatographed on silica
  8. washeluting with 0-10% methanol in ethyl acetate