HRID1285521

反应详情

EQUATION

反应方程式

HRID 1285521 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 147 mg (0.60 mmole) of cyclopropanoid cyanoester 10 (produced in accordance with Example VIII), 88 mg (0.64 mmole) of anhydrous potassium carbonate, 0.50 mL of water, and 2.0 mL of methyl alcohol was heated at reflux for 20 minutes. The product was isolated by cooling the mixture to room temperature, cautiously acidifying it by addition of 2 mL of 2M aqueous HCl, subsequent dilution with 20 mL of saturated brine, and extraction with ether. The ether extracts were washed with saturated brine, then dried over anhydrous magnesium sulfate and subsequently filtered. Removal of the ether by evaporation at reduced pressure afforded 110 mg (85% yield) of cyanoacid 18, which was immediately decarboxylated in accordance with Example XVI.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 20 minutes
  3. customThe product was isolated
  4. extractionwith 20 mL of saturated brine, and extraction with ether
  5. washThe ether extracts were washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationsubsequently filtered
  8. customRemoval of the ether
  9. customby evaporation at reduced pressure
  10. customafforded 110 mg (85% yield) of cyanoacid 18, which