HRID2077220

反应详情

EQUATION

反应方程式

HRID 2077220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-cyano-4-hydroxy-6-(2-methyl-benzothiazol-6-yloxy)-isoquinoline-3-carboxylic acid butyl ester (113 mg, 0.26 mmol) and glycine (390 mg, 5.20 mmol) in 0.5 M sodium methoxide/methanol (9.9 mL) was refluxed for forty-five hours before it was cooled to room temperature and concentrated in vacuo. The residue was dissolved in water (35 mL) and extracted with methyl tert-butyl ether (2×25 mL). The remaining aqueous layer was acidified to pH=3 with 1N HCl (7.4 mL). The white precipitate was filtered, washed with water and dried in vacuo to give the title compound as a white solid (92 mg): MS: (+) m/z 434.93 (M+1), (−) m/z 432.87 (M−1).

WORKUP

后处理

  1. temperaturewas refluxed for forty-five hours before it
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in water (35 mL)
  4. extractionextracted with methyl tert-butyl ether (2×25 mL)
  5. filtrationThe white precipitate was filtered
  6. washwashed with water
  7. customdried in vacuo