반응 #42497

반응 방정식

methyl 4-butyl-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylate

potassium hydroxide

→

title compound

수율 98.8%

4-Butyl-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylic acid

수율 98.8%

용매

methanol

반응 조건

후처리

1. 1
   농축concentrated under reduced pressure
2. 2
   workup.ADDITIONThe residue was diluted with water
3. 3
   세척washed with ethyl acetate
4. 4
   추출extracted with chloroform (4×50 mL)
5. 5
   건조The combined organic extracts were dried (sodium sulfate)
6. 6
   여과filtered
7. 7
   농축concentrated under reduced pressure

실험 절차

To a stirred solution of methyl 4-butyl-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylate (412 mg) in methanol (5 mL) was added 1 M potassium hydroxide (17 mL). The mixture was stirred at room temperature for 5 h and concentrated under reduced pressure. The residue was diluted with water and washed with ethyl acetate. The aqueous layer was acidified to pH 4 with 1 N hydrochloric acid and extracted with chloroform (4×50 mL). The combined organic extracts were dried (sodium sulfate), filtered, and concentrated under reduced pressure to provide 384 mg of the title compound: ESI MS m/z 236 [M+H]+.

출처