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Method for producing cyclopentyl sulfonyl chloride

A technology of cyclopentyl sulfonyl chloride and cyclopentyl mercaptan is applied in the field of preparation of cyclopentyl sulfonyl chloride, and can solve the problems of low yield, high product cost, low product purity and the like

Inactive Publication Date: 2008-07-16
XINXIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthetic method of existing sulfonyl chloride mainly contains mercaptan chlorine oxidation method, thiocyanate chlorination method and sodium thiosulfate chlorination method etc., but the shortcoming of these methods is that productive rate is lower, generally at 30-40%, Thereby the product cost is high, in addition, the purity of the product is on the low side, has been limited in the process of synthesizing pharmaceutical intermediates

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0006] Under the condition of 70°C, 2225ml of absolute ethanol was used as a solvent, 900ml of cyclopentyl chloride and 636 grams of sodium hydrosulfide were used as raw materials, and the reaction was carried out for 24 hours to prepare cyclopentylmercaptan. (2) Under strong stirring and dark conditions, 30ml Water is solvent, with 140g chlorine gas as oxidizing agent and reactant, oxidize 51g cyclopentyl mercaptan under the ice-salt bath cooling, strictly control the initial reaction temperature to be -5 ℃, when the reaction liquid is yellow-green, remove the ice-salt bath, Continue to introduce chlorine gas, and at the same time, naturally raise the temperature to 10°C. After the chlorine gas is passed, blow in air for 30 minutes, and at the same time, drop 3ml of 40% hydrogen peroxide. Pale yellow oil, after the lower organic phase was separated, it was transferred to a separatory funnel again, an equal volume of water and twice the volume of ether were added, and the liqui...

Embodiment 2

[0008] Under the condition of 75°C, 2225ml of absolute ethanol was used as a solvent, 900ml of cyclopentyl chloride and 636 grams of sodium hydrosulfide were used as raw materials, and the reaction was carried out for 48 hours to prepare cyclopentylmercaptan. Water is the solvent, with 140g of chlorine as the oxidant and reactant, oxidize 51g of cyclopentyl mercaptan under ice-salt bath cooling, and strictly control the early reaction temperature to 0°C. When the reaction solution is yellow-green, remove the ice-salt bath and continue Chlorine gas is passed through, and the temperature is naturally raised to 15°C. After the chlorine gas is passed through, air is blown in for 30 minutes, and 4ml of 40% hydrogen peroxide is dripped in at the same time. The yellow oil, after the lower organic phase was separated, was transferred to a separatory funnel again, an equal volume of water and twice the volume of diethyl ether were added, and the mixture was allowed to stand for liquid s...

Embodiment 3

[0010] Under the condition of 80°C, 2225ml of absolute ethanol was used as solvent, 900ml of cyclopentyl chloride and 636 grams of sodium hydrosulfide were used as raw materials, and cyclopentyl mercaptan was prepared by reacting for 72 hours. (2) under strong stirring and dark conditions, 30ml Water is the solvent, with 140g of chlorine as the oxidizing agent and reactant, oxidize 51g of cyclopentyl mercaptan under ice-salt bath cooling, and strictly control the initial reaction temperature at 5°C. When the reaction solution is yellow-green, remove the ice-salt bath and continue Chlorine gas is passed through, and the temperature is naturally raised to 20°C. After the chlorine gas is passed through, air is blown in for 30 minutes, and 5ml of 40% hydrogen peroxide is dripped in at the same time. The yellow oil, after the lower organic phase was separated, was transferred to a separatory funnel again, an equal volume of water and twice the volume of diethyl ether were added, and...

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Abstract

The invention discloses a preparation method for cyclopentyl sulfonyl chloride which relates to a preparation method for a derivative of sulfonic acid, aiming at providing a preparation method for the cyclopentyl sulfonyl chloride with high yield. The technique scheme of the invention is that the method for preparing the cyclopentyl sulfonyl chloride comprises the procedures of preparing a cyclopentyl mercaptan, and the cyclopentyl mercaptan, the water and a chlorine with a molar ratio of 1:3:4 are oxidated by avoiding light. Then the cyclopentyl mercaptan and the water are put in a flask, stirred and mixed evenly, then oxidated by pumping in the chlorine, with a chlorination temperature in the early phase of -10 to 5 DEG C. When the reaction liquid becomes yellowish green, the temperature is naturally raised to 10 to 20 DEG C, and the chlorine is pumped in continuously. When the pumping of chlorine is finished, air is blown into the flask and meanwhile, a hydrogen peroxide is dropped into the flask. When no chlorine is remained in the flask, the liquid is transferred in a separatory funnel to separate a lower layer organic phase and dried by a desiccant, after decompression and distillation, a colorless liquid of the production of cyclopentyl sulfonyl chloride is acquired. The invention is used for preparing the sulfonyl chloride.

Description

Technical field: [0001] The invention relates to a preparation method of sulfonic acid derivatives, in particular to a preparation method of cyclopentylsulfonyl chloride. Background technique: [0002] Sulfonyl chloride, as a series of organic synthesis raw materials, is mainly used as a chlorination agent for vat dyes, an assimilation agent for dry inks and dyes, and is also widely used as an intermediate in the synthesis of medicines and pesticides. The synthetic method of existing sulfuryl chloride mainly contains mercaptan chlorine oxidation method, thiocyanate chlorination method and sodium thiosulfate chlorination method etc., but the shortcoming of these methods is that productive rate is lower, generally at 30-40%, Thereby the product cost is high, in addition, the purity of the product is on the low side, has been restricted in the process of synthesizing pharmaceutical intermediates. Invention content: [0003] The purpose of this invention is to provide a kind ...

Claims

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Application Information

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IPC IPC(8): C07C309/85C07C303/16
Inventor 陈改荣苗郁陈永魁苗长庆应浩
Owner XINXIANG UNIV
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