반응 #45827

반응 방정식

Acetic acid

hydrochloric acid

tin chloride dihydrate

4-fluoro-2-methyl-6-nitrobenzonitrile

sodium hydroxide

→

compound

수율 104.9%

2-Amino-4-fluoro-6-methylbenzonitrile

수율 104.9%

용매

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타Since the reaction liquid
3. 3
   온도greatly generated heat
4. 4
   온도it was cooled with ice
5. 5
   여과The precipitated solid was collected by filtration
6. 6
   세척washed with water
7. 7
   기타dried

실험 절차

Acetic acid (16.0 ml, 28 mmol) was added to a concentrated hydrochloric acid (90 ml) solution of tin chloride dihydrate (63.1 g, 280 mmol), and 4-fluoro-2-methyl-6-nitrobenzonitrile (I-263) (16.8 g, 93.3 mmol) was added, then methanol (8 ml) was added. Since the reaction liquid greatly generated heat, it was cooled with ice. After stirring for 1 hour, the reaction mixture liquid was poured into aqueous sodium hydroxide solution (4.6 M, 500 ml) with ice therein. The precipitated solid was collected by filtration, washed with water, then dried to obtain the entitled compound (14.7 g, 99%) as a gray solid.

출처