HRID1469107

反应详情

EQUATION

反应方程式

HRID 1469107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.75 g of 4-chloro-6-iodoquinazoline, 0.58 g of 7-methoxy-1,2,3,4-tetrahydroisoquinoline and 0.64 ml of triethylamine in 5 ml of dioxane are heated at 80° C. in a flask until the quinazoline has reacted completely (HPLC check, about 2 hours). The cooled reaction solution is diluted with EA and washed 3 times with water. The organic phase is dried over sodium sulfate and purified by means of column chromatography (gradient heptane: EA 5-100% in 22 min.), giving 0.60 g of 6-iodo-4-(7-methoxy-3,4-dihydro-1H-isoquinolin-2-yl)quinazoline as yellowish solid (yield 57%, content 93%); MS-FAB (M+H+)=418.0; Rf (polar method): 1.87 min.

WORKUP

后处理

  1. customhas reacted completely (HPLC check, about 2 hours)
  2. customThe cooled reaction solution
  3. washwashed 3 times with water
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. custompurified by means of column chromatography (gradient heptane: EA 5-100% in 22 min.)