反应 #607466

反应方程式

Propanoyl chloride

anthranilic acid

hydrochloric acid

→

raw product

收率 78.2%

2-ethyl-4H-3,1-benzoxazin-4-one

收率 78.2%

溶剂

dichloromethane

反应条件

后处理

1. 1
   温度under reflux
2. 2
   其他After the end of the reaction
3. 3
   萃取the resulting mixture was extracted with ethyl acetate (100 mL)
4. 4
   干燥the extract was dried with magnesium sulfate
5. 5
   其他the solvent was evaporated
6. 6
   workup.ADDITIONAcetic anhydride (15 mL) was added to the residue
7. 7
   温度to reflux
8. 8
   其他After the end of the reaction
9. 9
   其他the reaction medium spin dried at a temperature of 65° C.

实验过程

Propanoyl chloride (6.2 g, 67 mmol) was added to a solution of anthranilic acid (1 g, 7.3 mmol) in dichloromethane (20 mL). The reaction medium was kept under reflux and agitation, with the end of the reaction being monitored by CG/MS. After the end of the reaction, a hydrochloric acid solution was added (20 mL, 1M), and the resulting mixture was extracted with ethyl acetate (100 mL), the extract was dried with magnesium sulfate and the solvent was evaporated. Acetic anhydride (15 mL) was added to the residue and the reaction medium was taken to reflux and accompanied through CG/MS in order to monitor cyclization. After the end of the reaction, the reaction medium spin dried at a temperature of 65° C. using portions of toluene to facilitate the elimination of the anhydride. 1.0 g of the raw product 2-ethyl-4H-3,1-benzoxazin-4-one was obtained, which was used directly in the stage subsequent to reaction.

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