HRID2184784

反应详情

EQUATION

反应方程式

HRID 2184784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl isocyanoacetate (2.19 g, 19.4 mmol) and allyl 2-bromo-2-methylpropionate (4.40 g, 21.3 mmol) are dissolved in diethyl ether (50 mL) and methyl sulfoxide (50 mL) with stirring. In a separate flask sodium hydride (775 mg of 60% dispersion in mineral oil) is rinsed with hexane and suspended in diethyl ether (10 mL). The suspension is added dropwise to the stirring solution and an additional methyl sulfoxide (50 mL) is added to the mixture. The reaction is stirred for 2 hours at room temperature. The mixture is diluted with diethyl ether (250 mL) and washed several times with water. The organic phase is dried over sodium sulfate and evaporated to give 3-isocyano-2,2-dimethyl-succinic acid 1-allyl ester 4-ethyl ester.

WORKUP

后处理

  1. washIn a separate flask sodium hydride (775 mg of 60% dispersion in mineral oil) is rinsed with hexane
  2. additionThe suspension is added dropwise to the stirring solution
  3. additionan additional methyl sulfoxide (50 mL) is added to the mixture
  4. additionThe mixture is diluted with diethyl ether (250 mL)
  5. washwashed several times with water
  6. dry with materialThe organic phase is dried over sodium sulfate
  7. customevaporated