반응 #833562

반응 방정식

tert-butyl N′-(quinolin-2-yl)methylene-hydrazinecarboxylate

→

Tert-butyl N′-(quinolin-2-ylmethyl)-hydrazinecarboxylate

용매

methanol

반응 조건

후처리

1. 1
   기타Then the precipitate and the catalyst are separated from the solvent
2. 2
   workup.DISSOLUTIONthe precipitate is dissolved in tetrahydrofuran
3. 3
   여과filtered again and in this way the catalyst
4. 4
   기타is separated off
5. 5
   기타The THF solution is evaporated down
6. 6
   기타the residue is triturated with tert-butylmethylether
7. 7
   기타separated off
8. 8
   기타dried at 50° C
9. 9
   기타The tert-butylmethylether phase is evaporated down again
10. 10
    기타the residue is triturated this time with diethyl ether
11. 11
    기타separated off
12. 12
    기타dried at 50° C
13. 13
    기타The two solid fractions from the purification with tert-butylmethylether and diethyl ether

실험 절차

0.5 g 10% Pd/C are added to a solution of 15.00 g tert-butyl N′-(quinolin-2-yl)methylene-hydrazinecarboxylate in 200 ml of methanol. The resulting mixture is then shaken for 6 h at ambient temperature under 1 atm H2 pressure. Then the precipitate and the catalyst are separated from the solvent, the precipitate is dissolved in tetrahydrofuran, filtered again and in this way the catalyst is separated off. The THF solution is evaporated down and the residue is triturated with tert-butylmethylether, separated off and dried at 50° C. The tert-butylmethylether phase is evaporated down again and the residue is triturated this time with diethyl ether, separated off and dried at 50° C. The two solid fractions from the purification with tert-butylmethylether and diethyl ether are combined.

출처