HRID1948603

反应详情

EQUATION

反应方程式

HRID 1948603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[8-(3-fluorophenyl)-1,4-dioxa-spiro[4.5]dec-8-yl]-dimethylamine hydrochloride (7.2 g, 22.75 mmole) was dissolved in water (9.6 ml), conc. hydrochloric acid (14 ml, 455 mmole) was added and the mixture was stirred for 4 days at room temperature. After completion of the hydrolysis the reaction mixture was extracted with diethyl ether (2×50 ml), the aqueous phase was make alkaline with 5N sodium hydroxide solution while cooling with ice, whereupon the product precipitated out. The ketone Ket-7 was isolated as a yellow solid with a melting point of 83°-88° C. and in a yield of 50% (6.05 g).

WORKUP

后处理

  1. customAfter completion of the hydrolysis the reaction mixture
  2. extractionwas extracted with diethyl ether (2×50 ml)
  3. temperaturewhile cooling with ice, whereupon the product
  4. customprecipitated out