3. 将苯乙酸甲酯 (50g, 0.33mol)、二氯甲烷 (66 m

3. phenylacetate (50g, 0.33mol), methylene chloride (66 mL) in a dry reaction flask, 0 ℃ with vigorous stirring, was slowly added dropwise fuming nitric acid (104g, 1.65mol) and dichloromethane ( 66mL) solution. After the dropwise addition was raised to room temperature and stirring continued for 1 h, TLC monitored the reaction. After completion of the reaction the reaction solution was washed with water until neutral, the organic phase was washed with a sodium sulfate solution (10%), and concentrated under reduced pressure to give a pale yellow liquid was fractionated Intermediate 2 (41.4g, 64%), bp 112 ~ 116 ℃.

3. Place phenythal (50g, 0.33mol), dichloromethane (66 mL) in a drying reaction bottle, stirring vigorously at 0C, slowly dripping with niactic acid (104g, 1.65mol) and dichloromethane (66mL) solution. After the drips are added, they are added and then raised to room temperature for 1 hour to continue stirring, the TLC monitors the reaction. After the reaction is completed, the water washing reaction fluid to neutral, organic phase with sodium sulfate solution (10%) wash, concentrated, decompression fractionation of pale yellow liquid for intermediate 2 (41.4g, 64%), b.p. 112 to 116 degrees C.

3. Put methyl phenylacetate (50g, 0.33mol) and dichloromethane (66ml) in a dry reaction bottle, stir vigorously at 0 ℃, and slowly add fuming nitric acid (104g, 1.65mol) and dichloromethane (66ml) solutions. After dropping, the mixture was stirred for 1 hour at room temperature, and TLC was used to monitor the reaction. After the reaction, wash the reaction solution with water to neutral, wash the organic phase with sodium sulphate solution (10%), concentrate, decompress and fractionate to obtain the light yellow liquid as intermediate 2 (41.4g, 64%), B.P. 112 ~ 116 ℃.<br>