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Preparation method of oxamide

A technology for oxamide and amine compounds, applied in the field of preparation of oxamide, can solve problems such as no industrial report, immature technology, etc., and achieve the effects of excellent substrate practicability, simple preparation process and high atomic economic benefit

Active Publication Date: 2019-07-23
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is still in the research stage and the technology is immature
[0008] In addition, the method for the oxidative carbonylation of CO and amine to synthesize oxamide derivatives can only be realized in a homogeneous palladium complex catalytic system (see: WO 2010 / 130696AI; CN 201080021316.9 and references I.Pri-Bar, H. Alper, Can.J.Chem., 1990,68,1544-1547), this method still has problems such as catalyst recycling, product separation, does not see relevant industrialization report

Method used

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  • Preparation method of oxamide
  • Preparation method of oxamide
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preparation example Construction

[0034] 1. Preparation of catalyst

[0035] The preparation method of catalyst among the present invention is example with the preparation process of catalyst 1-6, and 1-3 is the preparation technology of catalyst 1, and 4-12 is the preparation technology of catalyst 2, is embodied as follows:

Embodiment 1

[0036] Embodiment 1: Catalyst 1-1

[0037] Weigh 2.13g copper nitrate pentahydrate and 3.22g anhydrous palladium chloride, add to a round bottom flask, add 20wt% NH 4The OH solution was completely dissolved, and 15 g of pseudo-boehmite was added, and stirred at room temperature for 2 h. Afterwards, filter with suction, wash with distilled water until neutral, dry at 120°C for 12 hours, roast in a muffle furnace at 450°C for 3 hours, grind and sieve (80-100 mesh), and obtain the active catalyst 1-1 provided by the present invention.

Embodiment 2

[0038] Embodiment 2: Catalyst 1-2

[0039] Weigh 2.13g copper nitrate pentahydrate, 3.22g anhydrous palladium chloride, 15g pseudoboehmite, add to a round bottom flask, add 20mL distilled water to stir the solution to disperse, use 10wt% NaOH solution as precipitant for precipitation, and precipitate to pH About 10, heat up to 80°C for aging for 4h. After cooling down, filter with suction, wash with distilled water until neutral, dry at 120°C for 12 hours, roast in a muffle furnace at 450°C for 3 hours, grind and sieve (80-100 mesh), and then obtain the active catalyst 1-2 provided by the present invention.

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Abstract

The invention provides a preparation method of oxamide. The preparation method comprises the following steps: an intermediate oxamide derivative is prepared from CO, O2 and amine compounds as raw materials by oxidation and carbonylation under the action of a catalyst 1, and then, oxamide is prepared through aminolysis of the oxamide derivative under the action of a catalyst 2. A novel method is used for coproducing oxamide and the oxamide derivative, and the problems that oxalate synthesis materials are poisonous, catalyst efficiency is low and the like in the original technology for synthesizing oxamide through aminolysis of oxalate are solved. Besides, the technologically synthesized oxamide derivative has good substrate applicability and can be applied to fields of medicine, pesticides,synthetic ligands, food additives and the like.

Description

technical field [0001] The invention belongs to the technical field of oxamide synthesis, in particular to a preparation method of oxamide. Background technique [0002] Oxamide, also known as oxalic acid diamide, oxalamide, oxalamide, oxalamide (CAS No. 471-46-5), as a compound with high nitrogen content, is widely used in agriculture Fertilizer field. Oxamide is non-toxic, easy to store, and has low solubility, which makes it perform better than other fertilizers. For example, oxamide gradually decomposes and releases ammonia and carbon dioxide during the biodegradation process, which is harmless to the environment; the use of oxamide can improve the utilization rate of chemical fertilizers, reduce the frequency of fertilization, and reduce the harm to water resources; using oxamide as fertilizer It can reduce the cost of chemical fertilizers, manpower and time in the agricultural production process, which has been confirmed in the existing agricultural practice (see ref...

Claims

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Application Information

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IPC IPC(8): C07C231/10C07C233/56C07D295/182
CPCC07C231/10C07D295/182C07C233/56
Inventor 李跃辉常宇钰
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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