HRID1763715

反应详情

EQUATION

反应方程式

HRID 1763715 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.5 G. of 2-(5-oxo-5H-dibenzo[a,d]cyclohepten-2-yl)propionyl chloride is dissolved in 25 ml. of acetonitrile containing 0.5 ml. of allyl alcohol and 0.5 ml. of triethylamine. After 16 hours the mixture is evaporated to dryness and partitioned between ethyl acetate and water. The organic solution is washed, dried, passed through a short (10 g.) silica gel column, then evaporated to give allyl 2-(5-oxo-5H-dibenzo[a,d]cyclohepten-2-yl)propionate as an oil [nmr spectrum in deuterochloroform relative to tetramethylsilane: 1.54 (doublet, CH3), 2.84 (quartet, CH), 4.55 (doublet, OCH2), 5.1-6.0 (multiplet, CH=CH2) and 7.00 ppm (singlet, 10, 11-H); mass spectrum: 318(M+) 233,205].

WORKUP

后处理

  1. customAfter 16 hours the mixture is evaporated to dryness
  2. custompartitioned between ethyl acetate and water
  3. washThe organic solution is washed
  4. customdried
  5. customevaporated