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A kind of preparation method of o-methylisourea sulfate

A technology of methyl isourea and sulfate is applied in the preparation of urea derivatives, the preparation of organic compounds, chemical instruments and methods, etc., to achieve the effects of being conducive to environmental protection, less waste, and high yield

Active Publication Date: 2017-09-05
HUNAN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

By-product calcium sulfate is used as raw material for cement production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 63g (0.5moL) dimethyl sulfate to the three-necked flask, heat to 60°C, add 45g (0.75moL) urea at this temperature, then add 14.4g (0.8moL) water and 25.5g (0.25moL) concentrated sulfuric acid , at this temperature, keep warm for 4 hours; add 130g water to the reaction, cool down to 20°C, add 37g (0.5moL) calcium hydroxide, keep warm for 3 hours, filter, add 50mL methanol to the reaction for recrystallization. 55.5 g of O-methylisourea sulfate was obtained, with a content of 99.1%, and a total yield of 89.4% (in terms of dimethyl sulfate).

Embodiment 2

[0016] Add 63g (0.5moL) dimethyl sulfate to the three-necked flask, heat to 60°C, add 30g (0.5moL) urea at this temperature, then add 14.4g (0.8moL) water and 25.5g (0.25moL) concentrated sulfuric acid , at this temperature, keep warm for 4 hours; add 130g water to the reaction, cool down to 20°C, add 37g (0.5moL) calcium hydroxide, keep warm for 3 hours, filter, add 50mL methanol to the reaction for recrystallization. Obtain 50 g of O-methylisourea sulfate, the content is 99%, and the total yield is 80.5% (calculated by dimethyl sulfate).

Embodiment 3

[0018] Add 63g (0.5moL) dimethyl sulfate to the there-necked flask, heat to 60°C, add 60g (1moL) urea at this temperature, then add 14.4g (0.8moL) water and 25.5g (0.25moL) concentrated sulfuric acid, At this temperature, keep warm for 4 hours; add 130g of water to the reaction, cool down to 20°C, add 37g (0.5moL) of calcium hydroxide, keep warm for 3 hours, filter, add 50mL of methanol to the reaction for recrystallization. Obtain 55.3 g of O-methylisourea sulfate, the content is 99%, and the total yield is 89% (calculated by dimethyl sulfate).

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Abstract

The invention discloses a preparation method of O-methyl isourea sulphate. Reaction is divided into two process, a first process comprises the steps of adding urea and dimethyl sulphate into a reactor, mixing, then adding water and sulphuric acid, and carrying out reaction in the first process; and a second process comprises the steps of directly adding calcium hydroxide solid into a reaction liquid obtained in the first process in the reactor for carrying out reaction in the second process, and adding methyl alcohol after the reaction in the second process is completed for carrying out recrystallization, and filtering, so that the product O-methyl isourea sulphate is obtained. The total yield of the reactions in the two processes is more than 80%, and mass content of the product O-methyl isourea sulphate is more than 98%. The preparation method of the O-methyl isourea sulphate has the advantages that the reaction process is a 'quasi-one pot method' reaction, technology is simple, raw materials are available, solvent usage amount is small, operation is easy and yield is high; meanwhile, calcium hydroxide is adopted as the catalyst, fewer three wastes are produced in a preparation process, and environmental protection is facilitated; and a byproduct calcium sulphate can be applied to cement production, and comprehensive cost is further reduced, thereby being applicable to industrialized production.

Description

technical field [0001] The invention relates to a preparation method of O-methylisourea sulfate. Background technique [0002] O-methylisourea sulfate, molecular weight 246.24, white crystal, melting point 147-153°C, insoluble in methanol. As an intermediate, it is widely used in the fields of pesticide, medicine and biochemical synthesis, and is an important intermediate for the synthesis of fluorouracil antineoplastic drugs such as colon cancer, herbicides, and imidazole insect repellent pesticides. [0003] According to literature patent report, the method of main synthetic O-methylisourea sulfate at home and abroad at present is as follows: [0004] (1) Urea method: use dimethyl sulfate and urea as raw materials, recrystallize through ethanol, filter to obtain O-methylisourea bisulfate solid, and then add alkali to the reaction to obtain O-methylisourea sulfate. [0005] (2) Lime nitrogen method: Lime nitrogen is used as raw material to prepare O-methylisourea bisulfat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C273/00C07C275/70
CPCC07C273/00C07C275/70
Inventor 程超黄超群杜升华孔晓红兰世林
Owner HUNAN CHEM RES INST
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