HRID902744

反应详情

EQUATION

反应方程式

HRID 902744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

NaH (440 mg of a 60% dispersion in mineral oil, 11 mmole) was washed free of mineral oil, and suspended in 20 mL of DMF. This was treated with a solution of diethyl phenylmalonate (2.36 g, 10 mmole) in 10 mL of DMF, and the reaction was stirred for 15 minutes, at which time the solution was clear. 2-Methylallyl bromide (2.0 mL) was added, and stirring continued for 1 hour. The reaction was diluted with H2O and extracted with Et2O. The extracts were washed with H2O, dried and the solvent removed and gave the titled compound, 2.85 g (95% yield). MS (ESI) 291 (MH+)

WORKUP

后处理

  1. washNaH (440 mg of a 60% dispersion in mineral oil, 11 mmole) was washed free of mineral oil
  2. stirringstirring
  3. waitcontinued for 1 hour
  4. extractionextracted with Et2O
  5. washThe extracts were washed with H2O
  6. customdried
  7. customthe solvent removed