HRID1059423

反应详情

EQUATION

反应方程式

HRID 1059423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.32 g of (10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)methanol, 2.12 g of phthalimide and 3.77 g of triphenylphosphine in tetrahydrofuran (50 ml) was ice-cooled and 2.24 ml of diethyl azodicarboxylate was dropped thereinto. After stirring at room temperature for 1 hour, the solvent was distilled off under reduced pressure and diethyl ether was added to the residue. Then it was subjected to ultrasonication and the crystals thus precipitated were taken up by filtration to thereby give 2.6 g of the title compound as pale yellow crystals.

WORKUP

后处理

  1. temperaturecooled
  2. distillationthe solvent was distilled off under reduced pressure and diethyl ether
  3. additionwas added to the residue
  4. customThen it was subjected to ultrasonication
  5. customthe crystals thus precipitated
  6. filtrationwere taken up by filtration