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A temodar synthesis method

A technology of temozolomide and triethylamine, applied in the new synthesis field of temozolomide synthesis method, can solve problems such as unfavorable industrial production, difficult to grasp, explosion and the like

Active Publication Date: 2006-02-08
JIANGSU TASLY DIYI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As in the reaction of sodium nitrite and AIC.H 2 O, that is, 4-amino-5-carbamoyl imidazole monohydrate, etc., the reaction dosage range is too wide, it is difficult to grasp in the actual production operation, thus making the yield of the product unstable
[0006] Diazonium salt compound, the method of heating and drying in the refining process can easily cause explosion, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Synthesis of diazonium salt: Add 75g NaNO to a 3L three-necked flask 2 Stir with 1000ml of water to dissolve, and wash the mouth of the bottle with 500ml of water. Cool in an ice bath to 0°C, weigh 192ml (36.5%) of concentrated HCl and 95ml of water to prepare a 2N hydrochloric acid solution. Weigh 144.1 g of 4-amino-5-carbamoyl imidazole monohydrate (AIC) and dissolve it in 2N hydrochloric acid. The resulting AIC in 2N hydrochloric acid was added dropwise to NaNO 2 In the aqueous solution, the temperature is around 0-2°C. About 40 minutes to drip. After the dropwise addition, filter, wash with ethanol, 3 times, 300ml each time, and drain. The obtained light yellow solid was vacuum dried at 50° C. overnight. 124 g of light yellow solid was obtained with a yield of 90.5%.

[0026] 2. Synthesis of methyl isocyanate: Weigh 100g of methylcarbamoyl chloride into a 500mL four-necked bottle, add 80mL of toluene and stir to dissolve, cool down to 5°C, start adding trie...

Embodiment 2

[0031] 1. Synthesis of diazonium salt: Add 75g NaNO to a 3L three-necked flask 2 Stir with 1000ml of water to dissolve, and wash the mouth of the bottle with 350ml of water. Cool in an ice bath to 0°C, weigh 192ml (36.5%) of concentrated HCl and 95ml of water to prepare a 2N hydrochloric acid solution. Weigh 144.1 g of 4-amino-5-carbamoyl imidazole monohydrate (AIC) and dissolve it in 2N hydrochloric acid. The resulting AIC in 2N hydrochloric acid was added dropwise to NaNO 2 In the aqueous solution, the temperature is around 0-2°C. About 35 minutes to drip. After the dropwise addition, filter, wash with ethanol, 3 times, 300ml each time, and drain. The obtained light yellow solid was vacuum dried at 50° C. overnight. 124 g of a light yellow solid was obtained with a yield of 88.5%.

[0032] 2. Synthesis of methyl isocyanate: Weigh 100g of methylcarbamoyl chloride into a 500mL four-necked bottle, add 80mL of toluene and stir to dissolve, cool down to 5°C, start adding tr...

Embodiment 3

[0037] 1. Synthesis of diazonium salt: Add 75g NaNO to a 3L three-necked flask 2 Stir with 1000ml of water to dissolve, and wash the mouth of the bottle with 500ml of water. Cool in an ice bath to 0°C, and take a 2N hydrochloric acid solution. Weigh 144.1 g of 4-amino-5-carbamoyl imidazole monohydrate (AIC) and dissolve it in 2N hydrochloric acid. The resulting AIC in 2N hydrochloric acid was added dropwise to NaNO 2 In the aqueous solution, the temperature is around 0-2°C. About 30 minutes to drip. After the dropwise addition, filter, wash with ethanol, 3 times, 300ml each time, and drain. The obtained light yellow solid was vacuum dried at 50° C. overnight. 124 g of light yellow solid was obtained with a yield of 89.7%.

[0038] 2. Synthesis of methyl isocyanate: Weigh 100g of methylcarbamoyl chloride into a 500mL four-neck bottle, add 70mL of toluene and stir to dissolve, cool down to 5°C, start to drop triethylamine / toluene (150mL triethylamine / 90mL Toluene) solutio...

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Abstract

The invention discloses a process for synthesizing Temozolomide, which realizes the parameter optimization for the existing technique, and overcomes the deficits of the conventional processes.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a new synthesis method of Temozolomide synthesis method. Background technique [0002] Temozolomide (Temozolomide) is an alkylating dosage form anticancer drug, pioneered by Can research ventures in the UK and developed by Schering-Plough. It was approved by the FDA in August 1999 and was approved for marketing in the United States, and it was also marketed in many European countries. It has broad-spectrum antitumor activity [L.H.Tsang, et al. Cancer Chemother Pharmacol. 27(1991): 342-346], especially against glioma (brain cancer) and melanoma (skin cancer). Temozolomide capsules have been approved in Europe and the United States for the treatment of malignant glioma. [0003] At present, there are many synthetic methods of temozolomide reported in China, but the main steps are to use 4-amino-5-carbamoyl imidazole monohydrate as raw material, and carry ou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04C07D235/00C07D257/00
Inventor 陈明范荣徐学宇杨国军范立君李旭
Owner JIANGSU TASLY DIYI PHARMA CO LTD
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