HRID544303

反应详情

EQUATION

反应方程式

HRID 544303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-(2-Aminophenyl)oxazolidine-2,4-dione hydrochloride (1 g., 4.37 mmoles) was taken into 15 ml. of glacial acetic acid. Sodium acetate (358 mg., 4.37 mmoles) was added and then, in a dropwise manner, acetic anhydride (449 mg., 0.41 ml., 4.37 mmoles). The reaction mixture was stirred at room temperature for 16 hours, poured into 50 ml. of water and extracted with three portions of ethyl acetate. The combined extracts were washed with two portions of water and then one of brine, dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo solids (0.72g.). Recrystallization from ethyl acetate gave purified 5-(2-acetamidophenyl)oxazolidine-2,4-dione in two crops (0.26 g., m.p. 197°-198° C.; m/e 234).

WORKUP

后处理

  1. additionpoured into 50 ml
  2. extractionof water and extracted with three portions of ethyl acetate
  3. washThe combined extracts were washed with two portions of water
  4. dry with materialone of brine, dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo solids (0.72g.)
  7. customRecrystallization from ethyl acetate
  8. customgave
  9. custompurified 5-(2-acetamidophenyl)oxazolidine-2,4-dione in two crops (0.26 g., m.p. 197°-198° C.; m/e 234)