반응 #70505

반응 방정식

Furan-2,3-dicarboxylic acid dimethyl ester

EtOH

hydrazine hydrate

→

title compound

5,6-Dihydro-furo[2,3-d]pyridazine-4,7-dione

용매

H2O

반응 조건

후처리

1. 1
   온도Heat
2. 2
   기타the reaction
3. 3
   온도to reflux for 5-6 h
4. 4
   온도Cool
5. 5
   농축concentrate in vacuo
6. 6
   기타to form a slurry
7. 7
   여과filter the precipitate
8. 8
   세척Wash with additional H2O
9. 9
   여과Transfer material from filter to a round bottom flask
10. 10
    workup.ADDITIONadd HCl (7.2 mL, 2N in H2O)
11. 11
    온도Heat
12. 12
    기타reaction mixture
13. 13
    온도to reflux for 4 h
14. 14
    온도Cool
15. 15
    여과filter the precipitate
16. 16
    세척washing with H2O

실험 절차

Furan-2,3-dicarboxylic acid dimethyl ester (1.6 g, 8.69 mmol) is added to EtOH (10 mL) and hydrazine hydrate (1.46 mL, 55% in water). Heat the reaction to reflux for 5-6 h. Cool and concentrate in vacuo to form a slurry. Dilute the material with additional H2O and filter the precipitate. Wash with additional H2O. Transfer material from filter to a round bottom flask and add HCl (7.2 mL, 2N in H2O). Heat reaction mixture to reflux for 4 h. Cool and filter the precipitate washing with H2O, to yield the title compound without further purification (930 mg, 70%)

출처