反应 #67939

反应方程式

nitric acid

compound 10

4-acetylamino-5-chloro-2-methoxy-benzoic acid methyl ester

→

11

收率 91.0%

4-Acetylamino-5-chloro-2-methoxy-3-nitro-benzoic Acid Methyl Ester

收率 91.0%

溶剂

EtOAc

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   其他After separating the organic phase
3. 3
   萃取the aqueous phase was extracted with EtOAc
4. 4
   洗涤The combined organic phases were washed with brine
5. 5
   干燥dried over MgSO4
6. 6
   浓缩concentrated
7. 7
   其他Drying under hv

实验过程

Fuming nitric acid (33 mL) was added dropwise at 20° C. to compound 10 (13.0 g, 0.05 mol) over 15 min. After stirring for an additional 10 min at that temperature, the mixture was poured into ice water and EtOAc (100 mL) was added. After separating the organic phase, the aqueous phase was extracted with EtOAc. The combined organic phases were washed with brine, dried over MgSO4 and concentrated. Drying under hv yielded 14.0 g (91%) of 11 as a beige solid. 1H NMR (300 MHz, DMSO-d6): δ 2.01 (s, 3H), 3.84 (s, 3H), 3.87 (s, 3H), 8.12 (s, 1H), 10.30 (s, 1H).

来源