反应 #10407

反应方程式

(3-chloro-2-cyclopropylamino-4,5-difluorobenzoyl)-hydrazinecarboxylic acid tert-butyl ester

potassium carbonate

triphosgene

tetrahydrofuran

→

title compound

(8-Chloro-1-cyclopropyl-6,7-difluoro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)carbamic acid tert-butyl ester

溶剂

ethyl acetate

反应条件

后处理

1. 1
   温度The reaction mixture is refluxed for 90 minutes
2. 2
   洗涤The organic layer is washed with water and brine
3. 3
   干燥dried over MgSO4
4. 4
   过滤filtered
5. 5
   浓缩The filtrate is concentrated under vacuum
6. 6
   其他purified via flash column chromatography (1:2 ethyl acetate/hexanes)

实验过程

To a solution of (3-chloro-2-cyclopropylamino-4,5-difluorobenzoyl)-hydrazinecarboxylic acid tert-butyl ester (Example 6c) (1.93 g, 5.34 mmol) in tetrahydrofuran (50 mL) is added potassium carbonate (3.69 g, 26.7 mol) and triphosgene (2.06 g, 6.95 mmol). The reaction mixture is refluxed for 90 minutes, cooled to room temperature, and diluted with ethyl acetate. The organic layer is washed with water and brine, then dried over MgSO4 and filtered. The filtrate is concentrated under vacuum and purified via flash column chromatography (1:2 ethyl acetate/hexanes) to afford the title compound (1.27 g). MS EI: m/z 386 (M+).

来源