HRID1086383

反应详情

EQUATION

反应方程式

HRID 1086383 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 74.0 g (0.489 mol) of N-(2-hydroxyethyl)-N-methylaniline in 100 mL of pyridine was treated dropwise with 55 g (0.54 mol) of acetic anhydride. The resulting mixture was heated at reflux for 10 hr, then cooled and poured onto 500 g of ice. The mixture was extracted three times with dichloromethane (3×100 mL), the combined extracts were dried using magnesium sulfate (MgSO4) and the solvent was evaporated. The residue was distilled at reduced pressure, producing 84.2 g of a slightly yellow oil, b.p. 107°-116° C. (0.4 mm).

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 10 hr
  3. temperaturecooled
  4. extractionThe mixture was extracted three times with dichloromethane (3×100 mL)
  5. customthe combined extracts were dried
  6. customthe solvent was evaporated
  7. distillationThe residue was distilled at reduced pressure
  8. customproducing 84.2 g of a slightly yellow oil, b.p. 107°-116° C. (0.4 mm)