HRID614534

反应详情

EQUATION

反应方程式

HRID 614534 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.00 g. of 5,6-Dimethoxy-3-hydroxymethylene oxindole, 2.5 g. acetic acid and 6.5 g. piperazine-N-carboxylic acid isobutyl ester (U.S. Pat. No. 3,635,979) in 40 ml. benzene was refluxed using a water separator to remove the water as it formed. After 20 minutes, 200 ml. benzene was added and the solution extracted with potassium carbonate and water. The benzene sollution was treated with magnesium sulfate and charcoal, filtered, concentrated and the residue crystallized from isopropyl alcohol and ether to give 5.50 g. product, m.p. 195°-197° C.

WORKUP

后处理

  1. customto remove the water as it
  2. customformed
  3. extractionthe solution extracted with potassium carbonate and water
  4. additionThe benzene sollution was treated with magnesium sulfate and charcoal
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customthe residue crystallized from isopropyl alcohol and ether
  8. customto give 5.50 g