تفاعل #607466

معادلة التفاعل

Propanoyl chloride

anthranilic acid

hydrochloric acid

→

raw product

المردود 78.2%

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

المردود 78.2%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux
2. 2
   أخرىAfter the end of the reaction
3. 3
   استخلاصthe resulting mixture was extracted with ethyl acetate (100 mL)
4. 4
   تجفيفthe extract was dried with magnesium sulfate
5. 5
   أخرىthe solvent was evaporated
6. 6
   workup.ADDITIONAcetic anhydride (15 mL) was added to the residue
7. 7
   درجة الحرارةto reflux
8. 8
   أخرىAfter the end of the reaction
9. 9
   أخرىthe reaction medium spin dried at a temperature of 65° C.

الإجراء التجريبي

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.

المصدر