HRID2268128

反应详情

EQUATION

反应方程式

HRID 2268128 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(2-Hydroxyethoxy)phenol (308 g; 2 mol) was taken up in a 5 L Erlnmeyer flask fitted with mechanical stirrer. Anhydrous acetone (4 L, dried over K2CO3), and potassium carbonate powder (290 g; 2.1 mol) were added, and the mixture was stirred vigourously. Acetic anhydride (207 ml; 2.2 mol) was added from an additional funnel slowly over a period of 1 hour. Stiiring was continued for 3 hours. TLC (CH2Cl2/MeOH:9:1, v/v) showed disapperence of starting material. The reaction mixture was filtered, solid washed thoroughly with acetone (1 L). The combined fractions was concentrated and purified by chromatography eluting with hexane and ethyl acetate (0% to 35% EtOAc; v/v). The product was obtained as a colorless viscous oil. Yield 258-264 gms (70-72%)

WORKUP

后处理

  1. customfitted with mechanical stirrer
  2. filtrationThe reaction mixture was filtered
  3. washsolid washed thoroughly with acetone (1 L)
  4. concentrationThe combined fractions was concentrated
  5. custompurified by chromatography
  6. washeluting with hexane and ethyl acetate (0% to 35% EtOAc; v/v)
  7. customThe product was obtained as a colorless viscous oil