HRID2261837

反应详情

EQUATION

反应方程式

HRID 2261837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 4-{[(2-fluoro-6-methyl-4-triisopropylsilanyloxy-phenyl)-methyl-amino]-methyl}-2-methyl-benzoic acid methyl ester (457 mg, 0.965 mmol) and tetrabutylammonium fluoride (2.0 mL of 1M in THF, 2.0 mmol) in THF (10 mL) is stirred at 0° C. for 20 minutes and then 2.0 mL of 1M HCl is added and the mixture is concentrated. The residue is portioned between ethyl acetate and brine. The layers are separated and the brine layer is extracted with ethyl acetate. The combined ethyl acetate layers are dried (MgSO4) and concentrated. The residue is purified on 40 g silica with ethyl acetate in heptane gradient (10% to 70%) to provide 233 mg (76%) of the titled compound as a glass. LC-ES/MS m/e 318.2 (M+1).

WORKUP

后处理

  1. concentrationthe mixture is concentrated
  2. customThe layers are separated
  3. extractionthe brine layer is extracted with ethyl acetate
  4. dry with materialThe combined ethyl acetate layers are dried (MgSO4)
  5. concentrationconcentrated
  6. customThe residue is purified on 40 g silica with ethyl acetate in heptane gradient (10% to 70%)