HRID1646616

反应详情

EQUATION

反应方程式

HRID 1646616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

9 g of (2-methyl-2-propenyl)-tributyl stannane, 5.25 g of 4-bromo indanone, 50 ml of dimethylformamide and 300 g of tetrakis phenyl phosphine palladium are heated to 125° C. under agitation for 45 minutes. After cooling, the mixture is poured into an iced solution of 7.5 g of potassium fluoride in 300 ml of water, agitated for 5 minutes and filtered on celite. The filtrate is extracted with isopropyl ether, dried and concentrated to dryness under reduced pressure. The residue is chromatographed on silica, eluting with a hexane-ethyl acetate mixture (8-2) and 4 g of expected product is recovered.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationfiltered on celite
  3. extractionThe filtrate is extracted with isopropyl ether
  4. customdried
  5. concentrationconcentrated to dryness under reduced pressure
  6. customThe residue is chromatographed on silica
  7. washeluting with a hexane-ethyl acetate mixture (8-2) and 4 g of expected product
  8. customis recovered