HRID1723308

反应详情

EQUATION

反应方程式

HRID 1723308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 0.47 g of 3-(1,3-dioxolan-2-yl)thiophene-2-sulfonamide in 20 ml of acetonitrile was added 0.52 g of phenyl(4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate and 0.3 ml of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). After stirring at ambient temperatures for two hours the solution was diluted to 50 ml with water and the pH was adjusted to 3 by the addition of hydrochloride acid. The resultant solution was extracted with methylene chloride and the methylene chloride phase was dried over magnesium sulfate, filtered and evaporated. Trituration of the residue with butyl chloride yielded 0.6 g of the product, m.p. 164°-166°. Infrared absorption spectra showed peaks at 1700, 1600 and 1550 cm-1, consistent for the desired structure. ##STR27##

WORKUP

后处理

  1. extractionThe resultant solution was extracted with methylene chloride
  2. dry with materialthe methylene chloride phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated