HRID727216

反应详情

EQUATION

反应方程式

HRID 727216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A suspension of 1.6 grams (0.005 mole) of 4-amino-2-methylsulfinyl-6-(2-chlorophenyl)-5,6,7,8-tetrahydroquinazoline (prepared as in Example 17) and 10 mL of aqueous 40% methylamine in 50 mL of ethanol is placed in a glass tube, which is then sealed. The sealed tube is heated at about 180° C. for 7 hours and then is cooled in an ice-bath and opened. The reaction mixture is concentrated under reduced pressure to a residue. The residue is stirred with an aqueous 10% potassium carbonate solution, and the resultant suspension is extracted with chloroform. The extract is dried with magnesium sulfate and filtered. The filtrate is concentrated under reduced pressure to a residue. The residue is subjected to column chromatography on silica gel, yielding 4-amino-2-methylamino-6-(2-chlorophenyl)-5,6,7,8-tetrahydroquinazoline.

WORKUP

后处理

  1. customis placed in a glass tube
  2. customwhich is then sealed
  3. temperatureis cooled in an ice-bath
  4. concentrationThe reaction mixture is concentrated under reduced pressure to a residue
  5. extractionthe resultant suspension is extracted with chloroform
  6. dry with materialThe extract is dried with magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate is concentrated under reduced pressure to a residue