반응 #10393

반응 방정식

4-(pyrrolidin-1-yl)-2-cyclopropylamino-5-fluorobenzoic acid ethyl ester

sodium hydroxide

→

title compound

수율 89.9%

2-Cyclopropylamino-5-fluoro-4-pyrrolidin-1-ylbenzoic acid

수율 89.9%

용매

ethyl acetate

methanol

tetrahydrofuran

반응 조건

후처리

1. 1
   온도cooled to room temperature
2. 2
   세척The organic layer is washed with 1N hydrochloric acid, water, and brine
3. 3
   건조The organic layer is dried over MgSO4
4. 4
   여과filtered
5. 5
   농축the filtrate concentrated

실험 절차

To a solution of 4-(pyrrolidin-1-yl)-2-cyclopropylamino-5-fluorobenzoic acid ethyl ester (Example 3e, 3.10 g, 10.4 mmol) in methanol (50 mL) and tetrahydrofuran (20 mL) is added 1N solution of sodium hydroxide (35 mL). The reaction mixture is stirred at 80° C. for 20 hours, cooled to room temperature, and diluted with ethyl acetate. The organic layer is washed with 1N hydrochloric acid, water, and brine. The organic layer is dried over MgSO4, filtered, and the filtrate concentrated to afford the title compound as a solid (2.47 g). MS CI: m/z 263 (M+).

출처