HRID1242064

反应详情

EQUATION

反应方程式

HRID 1242064 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-amino-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyran-3-carboxylic acid tert-butyl ester (6.0 g, 0.014 mol) in ethanol (100 ml) was added hydrazine-hydrate (1.4 ml, 0.029 mol). The mixture was stirred at reflux temperature for 1 h. The cooled reaction mixture was filtered and the solvent evaporated in vacuo. The residue was dissolved in diethyl ether (200 ml) and washed with water (100 ml), brine (100 ml), dried (Na2SO4), filtered and the solvent evaporated in vacuo affording 2.9 g (71%) of 2-amino-7-aminomethyl-4,7-dihydro-5H-thieno[2,3-c]pyran-3-carboxylic acid tert-butyl ester as an oil.

WORKUP

后处理

  1. temperatureat reflux temperature for 1 h
  2. customThe cooled reaction mixture
  3. filtrationwas filtered
  4. customthe solvent evaporated in vacuo
  5. dissolutionThe residue was dissolved in diethyl ether (200 ml)
  6. washwashed with water (100 ml), brine (100 ml)
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. customthe solvent evaporated in vacuo