反応 #833562

反応方程式

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

→

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

溶媒

methanol

反応条件

後処理

1. 1
   その他Then the precipitate and the catalyst are separated from the solvent
2. 2
   workup.DISSOLUTIONthe precipitate is dissolved in tetrahydrofuran
3. 3
   ろ過filtered again and in this way the catalyst
4. 4
   その他is separated off
5. 5
   その他The THF solution is evaporated down
6. 6
   その他the residue is triturated with tert-butylmethylether
7. 7
   その他separated off
8. 8
   その他dried at 50° C
9. 9
   その他The tert-butylmethylether phase is evaporated down again
10. 10
    その他the residue is triturated this time with diethyl ether
11. 11
    その他separated off
12. 12
    その他dried at 50° C
13. 13
    その他The two solid fractions from the purification with tert-butylmethylether and diethyl ether

実験手順

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.

出典