HRID279750

反应详情

EQUATION

反应方程式

HRID 279750 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4,6-dichloro-1,3,5-triazin-2-yl isocyanate (3.10 g, 16.2 mmol) in acetonitrile (15 ml) was contacted with 2-(chloromethyl)benzene sulfonamide (3.34 g, 16.2 mmol) and stirred for 20 hrs at 25°. The mixture was heated at 50° for 2 hrs, cooled and filtered to provide 3.86 g, mp 162°-170°, which was contacted with sodium methoxide (30 mmol) in methanol (60 ml) at 20°-25° for 16 hrs. Water (100 ml) was added and the mixture was filtered and neutralized by addition of hydrochloric acid. Filtration and drying gave 2.20 g of white solid, mp 150°-152° (dec.).

WORKUP

后处理

  1. temperatureThe mixture was heated at 50° for 2 hrs
  2. temperaturecooled
  3. filtrationfiltered
  4. customto provide 3.86 g, mp 162°-170°, which
  5. filtrationthe mixture was filtered
  6. additionneutralized by addition of hydrochloric acid
  7. filtrationFiltration
  8. customdrying