HRID1763080

反应详情

EQUATION

反应方程式

HRID 1763080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

[6,7-Dichloro-2-(3-chloro-2-butenyl)-2,3-dihydro-1-oxo-2-propyl-1H-inden-5-yl]succinic acid (7.9 g, 0.01764 mole) was combined with quinoline (70 ml) and copper powder (2.9 g), stirred under N2 at 130°-135° C. (internal) in an oil bath for 1/2 hour. The mixture was poured into ice water, acidified with hydrochloric acid and extracted with methylene chloride. The organic extracts were washed with dilute HCl, H2O, dried over MgSO4 and concentrated under vacuum. The residue was chromatographed on silica eluting with methylene chloride, tetrahydrofuran, acetic acid (100:1:1) to obtain 7 g of the product as an oil.

WORKUP

后处理

  1. extractionextracted with methylene chloride
  2. washThe organic extracts were washed with dilute HCl, H2O
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under vacuum
  5. customThe residue was chromatographed on silica eluting with methylene chloride, tetrahydrofuran, acetic acid (100:1:1)