HRID1084874

反应详情

EQUATION

反应方程式

HRID 1084874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 3-methyl-4-hydroxy-5-tert-butyl-7-p-chlorobenzoylbenzofuran-2-carboxylate, compound 17 (0.322 g, 0.79 mmol) was suspended in a solution of potassium hydroxide (0.151 g, 2.69 mmol) in water (15 mL) and heated to reflux for 2.5 hours. The resulting solution was cooled in an ice bath and acidified with 2N HCl. The product precipitated and 3-methyl-4-hydroxy-5-tert-butyl-7-p-chlorobenoylbenzofuran-2-carboxylic acid, compound 18 was collected by filtration and allowed to air dry. mp 214°-216° C.; 1H NMR (DMSO-d6) d 1.44 (9H, s), 2.78 (3H, s), 5.78 (1H, s), 7.6 (2H, d, J=8 Hz), 7.62 (1H, s), 7.74 (2H, d, J=8 Hz).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 2.5 hours
  3. temperatureThe resulting solution was cooled in an ice bath
  4. customThe product precipitated
  5. filtration3-methyl-4-hydroxy-5-tert-butyl-7-p-chlorobenoylbenzofuran-2-carboxylic acid, compound 18 was collected by filtration
  6. customto air dry