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Process for preparing 2,2-di-[4-(3-nitro phenoxy) phenyl] propane

A technology of nitrophenoxy and m-dinitrobenzene, which is applied in two fields, can solve problems such as unsatisfactory industrialization prospects, and achieve the effects of reduced toxicity, low price, and improved operating environment

Inactive Publication Date: 2003-06-25
SHANGHAI RES INST OF SYNTHETIC RESINS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, although the above-mentioned method has solved the condensation etherification problem between the less reactive compound (m-dinitrobenzene) and alcohols or phenolic compounds, from the consideration of economic security, its industrialization prospect is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 22.8 grams (0.1 moles) of bisphenol A (BPA), 33.6 grams (0.2 moles) of m-nitrobenzene, 27.6 grams (0.2 moles) of anhydrous potassium carbonate, 70 grams of N, N-dimethylformamide (DMF ), 30 gram toluene and 0.5 gram triethylamine (TEA) add together in the there-necked flask that nitrogen tube, thermometer, stirrer, reflux condenser are equipped, connect nitrogen, heat up, react 24 hours under reflux temperature, Cool to room temperature, filter to remove potassium nitrite, concentrate the mother liquor under reduced pressure, cool, precipitate, filter, and recrystallize with toluene to obtain 2,2-bis-[4-(3-nitrophenoxy)phenyl]propane ( 3-BAPOPP) 42.3 g (90% yield), melting point 111-113°C.

Embodiment 2

[0019] Except adding 53.8 grams of m-dinitrobenzene (0.32 moles), 6.1 grams of triethylamine, 100 grams of toluene, and 300 grams of N,N-dimethylformamide, other process steps, material proportions and reaction parameters are all the same Example 1. As a result, 45.1 g (96% yield) of 2,2-bis-[4-(3-nitrophenoxy)phenyl]propane was obtained, with a melting point of 111-113°C.

Embodiment 3

[0021] Except adding 48.3 grams of anhydrous potassium carbonate (0.35 moles), 10 grams of triethylamine, 300 grams of toluene, and 450 grams of N, N-dimethylformamide, other process steps, material ratios and reaction parameters are all implemented with Example 2. As a result, 43.3 g (92.1% yield) of 2,2-bis-[4-(3-nitrophenoxy)phenyl]propane was obtained, with a melting point of 111-113°C.

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Abstract

The present invention relates to the preparation process of 2,2-di-[4-(3-nitro phenoxy) phenyl] propane. Under the action of anhydrous potassium carbonate as salt forming agent, N,N-dimethyl formamide as solvent, toluene as dewatering agent and triethylamine as catalyst, bisphenol A and m-dinitrobenzene are reflux reacted at 110-180 deg.c to prepare 2,2-di-[4-(3-amino phenoxy)phenyl] propane, which is purified through re-crystallization in toluene. The said process has 2,2-di-[4-(3-nitro phenoxy) phenyl] propane yield of 90-96%, and the product has smelting point of 111-113 deg.c.

Description

technical field [0001] The present invention relates to a preparation method of 2,2-bis-[4-(3-nitrophenoxy)phenyl]propane. Background technique [0002] 2,2-bis-[4-(3-nitrophenoxy)phenyl]propane (3-BNPOPP) is the preparation of 2,2-bis-[4-(3-nitrophenoxy)phenyl] Propane (3-BAPOPP) is an important raw material, and 3-BAPOPP is a rare and important raw material for the preparation of polyetherimide and polyarylamide, and it is also a good curing agent for impact-resistant epoxy resin. Therefore, the research and development of 2,2-bis-[4-(3-nitrophenoxy)phenyl]propane (3-BNPOPP) is particularly important. [0003] Patent Publication No. 54-39030 of the prior art discloses a method for preparing 3-nitrodiphenyl ether compound by utilizing m-dinitrobenzene and alkali metal phenoxide. It is prepared by reacting m-dinitrobenzene and alkali metal phenate under the action of polar solvent and macrocyclic polyether to prepare 3-nitrodiphenyl ether compound. [0004] Special Public...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/38
Inventor 虞鑫海
Owner SHANGHAI RES INST OF SYNTHETIC RESINS
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