Process for the recovery of oxazole
A kind of technology of oxazole and oxazole acid, applied in the purification field of oxazole, can solve the problems such as oxazole is not easy to synthesize
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Embodiment 1
[0060] In a 250ml round bottom flask, drop in a 100g (gram) mixture sample consisting of 11wt% oxazole, 1.67wt% HCN, 16wt% water, 12wt% acrylonitrile, 1wt% methanol and the balance acetonitrile Add 33.63g (0.34mol) of concentrated sulfuric acid. Form two layers. The aqueous layer containing greater than 99% of the oxazole in the oxazolium hydrogensulfate form was decanted from the organic layer. The aqueous layer was then extracted three times with 35 ml (milliliter) portions of dichloromethane in a 125 ml separatory funnel.
[0061] After extraction, the aqueous layer was added dropwise to a mechanically stirred slurry formed of 32 g (0.8 mol) NaOH in 21 g of water cooled to 10°C. Two layers are formed; the upper layer is mainly oxazole and the lower layer contains water and solid sodium sulfate decahydrate. The mixture was directly distilled. 9.94 g of crude oxazole were collected as a distillate between 68°C and 71°C. This distillate, containing 6 wt% water, was then s...
Embodiment 2
[0063] 50 g of the mixture as described in Example 1 was charged into a 100 ml three necked round bottom flask. The flask was equipped with a finger condenser, gas dispersion tube, glass stopper and magnetic stir bar. A drying tube containing a solid desiccant is connected to the condenser; the drying tube serves as a vent. The condenser was cooled to -78°C with a mixture of dry ice and acetone. The gas dispersion tube was connected to the demonstration bottle of HCl gas with a length of polyvinyl chloride tubing. The flow of HCl gas from the demonstration bottle was regulated with a manual control valve. The flask was immersed in an ice bath. After the mixture was cooled to 0°C, 5.33 g of HCl gas (0.146 mol) was bubbled into it. The mixture immediately separated into two layers.
[0064] The aqueous layer was separated from the organic layer, then extracted three times with 15 ml portions of dichloromethane in a 60 ml separatory funnel. After extraction, the aqueous lay...
Embodiment 3
[0066] In a 250ml three-necked flask equipped with a mechanical stirrer and two rubber septa, the mixture (112g) containing 32wt% oxazole, 2.86wt% of HCN, 15 wt% of water and the balance of acetonitrile. Form two layers. HCN was converted to NaCN and extracted into the lower aqueous layer and the upper organic layer contained less than 1 wt% water. The organic layer was decanted from the aqueous layer and distilled at ambient pressure. The mostly organic layer was distilled between 60°C and 92°C and had a composition of 43 wt% oxazole and balance acetonitrile. Concentrated sulfuric acid (51.5 g) was added dropwise to the distillate with good stirring in a three-necked flask equipped with a mechanical stirrer, addition funnel, and filter rod passed through the septum. An ice bath was used to maintain the temperature of the flask contents between 5°C and 20°C during the addition. Once formed, the oxazole sulfate precipitated immediately. After the acid addition was complete...
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