반응 #423612

반응 방정식

methyl ester

Methyl 4,6-dichloro-3-methoxy-2-nitrobenzoate

NaOH

→

acid 2-1

수율 94.1%

4,6-Dichloro-3-methoxy-2-nitrobenzoic acid

수율 94.1%

용매

MeOH

반응 조건

후처리

1. 1
   온도the reaction was heated
2. 2
   온도to reflux for 2.5 h
3. 3
   기타Methanol was removed in vacuo
4. 4
   추출the mixture was extracted with EtOAc
5. 5
   추출extracted into EtOAc (×3)
6. 6
   세척The combined organic layers were washed with brine
7. 7
   건조dried over Na2SO4
8. 8
   여과filtered
9. 9
   농축concentrated

실험 절차

To the methyl ester 2-2 (9.90 g, 35.3 mmol) in MeOH (150 mL) was added 2N NaOH (150 mL) and the reaction was heated to reflux for 2.5 h. Methanol was removed in vacuo and the mixture was extracted with EtOAc. The aqueous layer was acidified to pH 2 with a concentrated solution of HCl and then extracted into EtOAc (×3). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated to provide the acid 2-1 as an orange solid (8.84 g, 94% yield). 1H NMR (400 MHz, d6-DMSO) δ 3.83 (s, 3H), 3.95 (s, 3H), 8.23 (s, 1H).

출처