تفاعل #65639

معادلة التفاعل

compound

t-Butyl-2,3-dioxobutyrate

5,6-diamino-2,2-dimethyl-1,3-benzodioxole

dihydrochloride

NaOH

→

2,2,7-Trimethyl-1,3-dioxolo-[4,5-g]-quinoxaline-6-carboxylic acid, 1,1-dimethylethyl ester

المذيبات

water

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed for 2 hours
2. 2
   تركيزconcentrated in vacuo
3. 3
   أخرىto remove the organic solvent tetrahydrofuran
4. 4
   استخلاصextracted with ethyl acetate
5. 5
   غسيلThe combined organic phases were washed with brine
6. 6
   تجفيفdried (Na2SO4)
7. 7
   أخرىevaporated in vacuo
8. 8
   أخرىto leave an oil which
9. 9
   أخرىcrystallized by the addition of petroleum ether

الإجراء التجريبي

[5,6-diamino-2,2-dimethyl-1,3-benzodioxole; dihydrochloride salt] (U.S. Pat. No. 4,904,775, Example 3D) (6.8 g, 0.02 mmol) was dissolved in a mixture of 25 ml water and 10 ml tetrahydrofuran and the pH of the solution was adjusted to 5.5 by the addition of 2N NaOH. After addition of the compound from Example 1 (3.8 g; 0.02 mol) the mixture was refluxed for 2 hours, concentrated in vacuo to remove the organic solvent tetrahydrofuran and then extracted with ethyl acetate. The combined organic phases were washed with brine, dried (Na2SO4) and then evaporated in vacuo to leave an oil which crystallized by the addition of petroleum ether.

المصدر