2-acetyl thiophene synthetic method using thiophene in crude benzene as material

A technology for acetylthiophene and thiophene, applied in the field of synthesizing 2-acetylthiophene, can solve the problems of poor efficiency, complicated process, low recovery rate of thiophene, etc., to avoid the destruction of thiophene resources, simple process flow, and low recovery rate Effect

Inactive Publication Date: 2004-11-10
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Application Information

AI Technical Summary

Problems solved by technology

The catalytic hydrogenation method uses Co-Mo series hydrogenation catalysts to hydrogenate and saturate thiophene under the conditions of 350-400°C and 2.5-6.0MPa, and then convert it into hydrogen sulfide to achieve the purpose of desulfurization. The thiophene is destroyed and the resource cannot be recovered; sulfuric acid washing The process uses the sulfonation reaction of thiophene and sulfuric acid to convert thiophene into thiophenesulfonic acid, and then achieves the purpose of refining coking benzene. Although thiophenesulfonic acid can be further refined to obtain thiophene products after hydrolysis, this process is not only complicated and highly polluting , high consumption, the main disadvantage is that the recovery rate of thiophene is very low and the benefit is poor
[0007] Due to the above reasons, domestic thiophene resources are very scarce, and the production of thiophene pharmaceutical intermediates mainly depends on the current situation of importing foreign high-purity thiophene as raw materials.

Method used

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  • 2-acetyl thiophene synthetic method using thiophene in crude benzene as material

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Embodiment 1

[0019] Using coking light benzene containing 3350 mg / L thiophene as raw material, adopting the method introduced in the patent "A method for preparing pure benzene and concentrated thiophene from crude benzene" through one-stage and two-stage extraction and rectification to obtain thiophene containing 1.98% (by weight) respectively. ) and 19.5% (weight) of thiophene-benzene solution as raw material, with 85% phosphoric acid, Hβ zeolite molecular sieve, strongly acidic ion exchange resin, active clay, anhydrous zinc oxide, iron trichloride as catalyst, acetic anhydride is acetyl Chemical reagent, under the conditions of 40°C-90°C, normal pressure, and the molar ratio of acetic anhydride to thiophene is 2, convert thiophene into 2-acetylthiophene, the conversion rate of thiophene and the selectivity of 2-acetylthiophene of different catalysts See Table 1: Table 1 The reaction results of different catalysts catalyzing the synthesis of 2-acetylthiophene from thiophene and acetic an...

Embodiment 2

[0030] Adopting the benzene solution containing thiophene 19.5% involved in embodiment 1 as raw material, with 85% phosphoric acid, polyphosphoric acid, Hβ zeolite molecular sieve, strongly acidic ion exchange resin, anhydrous zinc chloride, iron trichloride as catalyst, Acetic anhydride is an acetylation reagent. It converts thiophene into 2-acetylthiophene under the condition of 40°C-90°C, normal pressure and the molar ratio of acetic anhydride to thiophene is 3. The conversion rate of thiophene and 2-acetylthiophene of different catalysts The selectivity of thiophene is shown in Table 2:

[0031] Table 2 Synthesis of 2-acetylthiophene from thiophene and acetic anhydride catalyzed by different catalysts

[0032] Catalyst Reaction temperature °C Material-dosage ratio * mass space velocity (h -1 ) Thiophene Conversion Rate 2-Acetylthiophene Selectivity (%)

[0033] (%)

[0034] 85% phosphoric acid 90 15 / >99.0 99.2

[0035] Po...

Embodiment 3

[0041] Using coked light benzene containing 4250mg / L thiophene as raw material, adopting the process introduced in the patent "A method for preparing pure benzene and concentrated thiophene from crude benzene" through two-stage extraction and rectification to obtain thiophene containing 24% (weight) thiophene - Benzene solution as raw material, with 85% phosphoric acid, Hβ zeolite molecular sieve, strong acid ion exchange resin, activated clay, anhydrous zinc chloride, ferric chloride as catalyst, acetic anhydride as acetylation reagent, at 40 ℃ -90 Under the conditions of ℃, normal pressure and the molar ratio of acetic anhydride and thiophene being 2, thiophene was converted into 2-acetylthiophene, the conversion rate of thiophene and the selectivity of 2-acetylthiophene of different catalysts are shown in Table 3:

[0042] Table 3 Synthesis of 2-acetylthiophene from thiophene and acetic anhydride catalyzed by different catalysts

[0043] Catalyst Reaction temperature °C Mat...

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Abstract

The invention provides a process for synthesizing 2- acetyl thiophene pharmaceutical intermediate compound by using thiophene in crude benzole through selective acetylation reaction, wherein an extraction and distillation method is adopted to condensate the thiophene in carbonized crude benzole, and to further prepare acetyl thiophene pharmaceutical intermediate compound from the thiophene concentrate through catalytic conversion.

Description

technical field [0001] The invention relates to the deep processing and utilization of crude benzene, a by-product produced in the industrial production process of iron and steel enterprises and coking enterprises. A method for further synthesizing 2-acetylthiophene from the thiophene concentrate obtained by distillation. Background technique [0002] 2-Acetylthiophene is an intermediate in the synthesis of a new broad-spectrum antibiotic, cephalosporin. The synthesis of 2-acetylthiophene both at home and abroad uses thiophene with high purity as raw material. Because high-purity thiophene is very expensive and the preparation process is complicated, the cost of such intermediates and broad-spectrum antibiotics synthesized from the intermediates is generally high. [0003] At present, the domestic method for synthesizing 2-acetylthiophene is mainly synthesized by industrial thiophene (content greater than 95%) and acetic anhydride under the catalysis of phosphoric acid, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/16
Inventor 罗国华
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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