HRID1375067

反应详情

EQUATION

反应方程式

HRID 1375067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (2-(4-(2-(2-o-tolylamino-benzoxazol-6-yl)-acetylamino)-phenyl)-indan-2-yl)-acetic acid ethyl ester [0.297 g, Reference Example 9(a)] in ethanol (10 mL) was treated with aqueous sodium hydroxide (1.61 mL, 1N) and the mixture was heated at reflux temperature for 6 hours and then left at room temperature overnight and then evaporated. The residue was treated with water (30 mL) and the resulting mixture was acidified to pH 1 by addition of hydrochloric acid (1N) then extracted with ethyl acetate. The ethyl acetate extract was dried over magnesium sulfate and then evaporated. The residue was dissolved in hot acetonitrile and the solution was treated with charcoal then filtered. The filtrate was evaporated to give the title compound (0.07 g) as a biscuit coloured solid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux temperature for 6 hours
  3. customevaporated
  4. additionThe residue was treated with water (30 mL)
  5. additionthe resulting mixture was acidified to pH 1 by addition of hydrochloric acid (1N)
  6. extractionthen extracted with ethyl acetate
  7. extractionThe ethyl acetate extract
  8. dry with materialwas dried over magnesium sulfate
  9. customevaporated
  10. dissolutionThe residue was dissolved in hot acetonitrile
  11. additionthe solution was treated with charcoal
  12. filtrationthen filtered
  13. customThe filtrate was evaporated