반응 #3200

반응 방정식

sodium hydroxide

5,7-dichloro-2H-3,1-benzoxazine-2,4(1H)-dione

→

methyl 2-amino-4,6-dichlorobenzoate

수율 92.2%

용매

methanol

반응 조건

후처리

1. 1
   온도to cool to room temperature
2. 2
   농축concentrated
3. 3
   workup.ADDITIONThe residue was diluted with water
4. 4
   추출the resulting mixture extracted with ethyl acetate
5. 5
   건조The combined extracts were dried (MgSO4)
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

To a stirred solution of sodium hydroxide (0.070 g, 1.8 mM) in methanol (8.5 mL) was added 5,7-dichloro-2H-3,1-benzoxazine-2,4(1H)-dione (4.13 g, 17.8 mM). The reaction mixture was stirred at 55° C. for 2 hr, allowed to cool to room temperature and concentrated. The residue was diluted with water and the resulting mixture extracted with ethyl acetate. The combined extracts were dried (MgSO4), filtered and concentrated to leave the methyl 2-amino-4,6-dichlorobenzoate (3.61 g, 92.1%) as a brown solid; MS(CI): 220 (M+H).

출처