Reaktion #577185

Reaktionsgleichung

hydrazine hydrate

product

3-chloro-1N-methyl-5-nitroindole-2-carboxylic acid ethyl ester

→

title compound

Ausbeute 100.3%

3-chloro-1N-methyl-5-amino-indole-2-carboxylic acid ethyl ester

Ausbeute 100.3%

Lösungsmittel

toluene

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe Raney Ni was removed by filtration through Celite
2. 2
   Sonstigethe solvent was removed in vacuo
3. 3
   Sonstigeto give the crude product
4. 4
   Einengenconcentrated in vacuo
5. 5
   workup.DISSOLUTIONThe residue was again dissolved in toluene (100 mL)
6. 6
   Einengenconcentrated in vacuo
7. 7
   Filtrationthe product was collected by filtration

Vorschrift

To a refluxing mixture of hydrazine hydrate (10.8 ml, 222 mmol) and Raney Ni (6 g) in MeOH (200 mL) was slowly added the product of step (b) (12.6 g), and the refluxing was continued for 6 hours. After cooling to room temperature, the Raney Ni was removed by filtration through Celite, and the solvent was removed in vacuo to give the crude product. The residue was dissolved in toluene (100 mL), and concentrated in vacuo. The residue was again dissolved in toluene (100 mL), and concentrated in vacuo, the residue was suspended in diethyl ether, and the product was collected by filtration to afford 11.3 g of the title compound.

Quelle