ChemicalBook CAS DataBase List 4-Aminophthalhydrazide

4-Aminophthalhydrazide synthesis

10synthesis methods

Product Name:4-Aminophthalhydrazide
CAS Number:3682-14-2
Molecular formula:C8H7N3O2
Molecular Weight:177.16

3682-19-7

3682-14-2

The general procedure for the synthesis of 4-amino phthalazine hydrazide using 6-nitro-2,3-dihydrophthalazine-1,4-dione as starting material was as follows: Intermediate B was transferred to a 5L high-pressure hydrogenation reactor and 3 g of 10% palladium/carbon catalyst was added. The reaction system was heated to 35 ℃ and hydrogen was introduced until the pressure reached 4 atm, and the reaction was maintained at a constant pressure for 4 h. After the reaction was completed, the reaction was carried out with nitrogen. Upon completion of the reaction, the hydrogen in the reactor was replaced with nitrogen. Subsequently, the pH of the reaction solution was adjusted to 3-4 with 35% by weight concentrated hydrochloric acid. heating was continued to 100°C and the nitrogen gas flow was stopped. The reaction mixture was filtered while hot and the filtrate precipitated a large amount of solid after cooling to room temperature. The solid precipitate was collected by filtration and the filtrate could be used for organic solvent recovery. The resulting filter cake was washed with 400 ml of deionized water and dried to give 214 g of 4-amino phthalic hydrazide (isluminolide).

3682-19-7 Synthesis

3682-19-7
72 suppliers
$60.00/100mg

3682-14-2
168 suppliers
$77.00/1g

Yield:3682-14-2 85%

Reaction Conditions:

with 10% Pd/C;hydrogen at 35; under 3040.2 Torr; for 4 h;

Steps:

1.3

Transfer the product B to a 5 L hydrogenation vessel, add 3 g of 10 wt% palladium on carbon palladium, heat to 35 ° C, while the introduction of hydrogen pressure to 4atm, continue to heat constant pressure reaction 4 hours, after the end of the reaction, the hydrogen into nitrogen, Adjust the pH to 3-4 with 35 wt% concentrated hydrochloric acid, continue heating to 100 ° C, stop the introduction of nitrogen, filter hot, and cool the filtrate to HTC, a large number of precipitated precipitation, precipitate out completely after the filter, the filtrate for organic solvent recovery, filter cake with 400ml deionized water washing, drying, to be 214g isluminolide (4-amino phthalide)

References:

CN106810501,2017,A Location in patent:Paragraph 0050

2307-00-8 Synthesis