반응 #423611

반응 방정식

phenol

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

acetone

K2CO3

iodomethane

→

methyl ester

수율 91.0%

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

수율 91.0%

용매

H2O

반응 조건

후처리

1. 1
   온도The flask was cooled
2. 2
   기타The volatiles were removed in vacuo
3. 3
   추출After extracting into CH2Cl2 (×3)
4. 4
   세척the combined organic layers were washed with H2O
5. 5
   건조dried over Na2SO4
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

To the phenol 1-7 (10.4 g, 39.1 mmol) in HPLC grade acetone (150 mL) was added K2CO3 (15 g, 108.5 mmol) and iodomethane (5 mL, 80.3 mmol). The reaction was heated to 60° C. for 22 h. The flask was cooled and then H2O (40 mL) was added and the mixture stirred for 30 min. The volatiles were removed in vacuo and the residue was taken up in CH2Cl2 and H2O. After extracting into CH2Cl2 (×3), the combined organic layers were washed with H2O, dried over Na2SO4, filtered and concentrated to give the methyl ester 2-2 as an orange oil (9.92 g, 91% yield). 1H NMR (400 MHz, d6-DMSO) δ 0.95 (s, 3H), 8.22 (s, 1H).

출처