HRID1721868

反应详情

EQUATION

反应方程式

HRID 1721868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Amino-N-[[(1-methylethyl)amino]carbonyl]-4-(methylthio)-5-pyrimidinesulfonamide (3.0 g, 9.84 mmol) was dissolved in dry (freshly distilled from sodium/benzophenone) THF (60 mL) and m-chloroperbenzoic acid (MCPBA) (2.55 g, 11.81 mmol, 80% 1.2 eq) was added as a solid. The reaction turned yellow and a white solid precipitated out of solution. After 30 minutes the reaction was diluted with ethyl ether (60 mL) and the white solid was filtered, washed with THF, then with ether three times and air dried for 2 hours, to yield 2.64 g (8.22 mmol, 84%) of product, m.p. 140° C.(dec.). The product was unstable to heat but could be stored under nitrogen in the freezer for weeks.

WORKUP

后处理

  1. customin dry (
  2. additionwas added as a solid
  3. customa white solid precipitated out of solution
  4. additionAfter 30 minutes the reaction was diluted with ethyl ether (60 mL)
  5. filtrationthe white solid was filtered
  6. washwashed with THF
  7. dry with materialwith ether three times and air dried for 2 hours