反应 #833562

反应方程式

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

→

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

溶剂

methanol

反应条件

后处理

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

实验过程

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.

来源