تفاعل #3206

معادلة التفاعل

sodium hydroxide

5,7-dimethyl-2H-3,1-benzoxazine-2,4(1H)-dione

→

title compound

المردود 86.0%

Methyl 2-amino-4,6-dimethylbenzoate

المردود 86.0%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةmaintained at that temperature for 45 min during which vigorous gas evolution
2. 2
   workup.DISSOLUTIONall solids dissolved completely
3. 3
   درجة الحرارةThe solution was cooled
4. 4
   تركيزconcentrated
5. 5
   أخرىa rotary evaporator
6. 6
   workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
7. 7
   غسيلthe ethyl acetate solution was washed with water
8. 8
   أخرىdried (Na2 SO4)
9. 9
   ترشيحfiltered
10. 10
    تركيزconcentrated

الإجراء التجريبي

To a stirred solution of sodium hydroxide (0.013 g, 0.33 mM) in methanol (1.7 mL) was added 5,7-dimethyl-2H-3,1-benzoxazine-2,4(1H)-dione (0.67 g, 3.5 mM). The mixture was heated to 60° C. and maintained at that temperature for 45 min during which vigorous gas evolution ensued and all solids dissolved completely. The solution was cooled and concentrated using a rotary evaporator. The residue was dissolved in ethyl acetate, and the ethyl acetate solution was washed with water, dried (Na2 SO4), filtered and concentrated to provide the title compound (0.54 g, 86%) as a tan solid; MS(CI); 180 (M+H).

المصدر