Preparation method of 4-amino-7-iodopyrrolo [2, 1-f] [1, 2, 4] triazine
A technology of aminopyrrole and amino, which is applied in the field of preparation of 4-amino-7-iodopyrrolo[2,1-f][1,2,4]triazine, can solve the problem of low product purity, difficult removal, di Problems such as high content of iodide impurities and isomer impurities, etc., to achieve the effect of high product yield, easy availability of raw materials, and high purity
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Embodiment 1
[0038] A preparation method of 4-amino-7-iodopyrrolo[2,1-f][1,2,4]triazine, comprising the following steps:
[0039] 1) Under nitrogen protection, add 80g (0.6mol) of 4-aminopyrrolo[2,1-f][1,2,4]triazine into 400mL of N,N-dimethylformamide and stir well , lower the temperature to -25°C, add 181.8g (0.716mol, 1.2equiv) of iodine in equal amounts in batches, and react at -10°C for 3h after feeding is complete;
[0040] 2) Add 80 mL (1.35 mol) of acetic acid and 60 g (0.24 mol, 0.4 equiv) of N-iodosuccinimide in batches to the reaction solution in step 1), and react at -10°C for 1 h;
[0041] 3) Mix and stir 225.7g (1.791mol, 3equiv) of sodium sulfite, 101.2g (0.955mol, 1.6equiv) of sodium carbonate and 2000mL of water evenly, cool down to 5°C to obtain an alkali solution, and slowly add the alkali solution dropwise Into the reaction solution of step 2), adjust the pH of the system to 9 with saturated sodium carbonate solution after adding, stir for 2 hours, filter, the filtered...
Embodiment 2
[0043] A preparation method of 4-amino-7-iodopyrrolo[2,1-f][1,2,4]triazine, comprising the following steps:
[0044] 1) Under nitrogen protection, add 900g (6.71mol) of 4-aminopyrrolo[2,1-f][1,2,4]triazine into 4000mL of N,N-dimethylformamide and stir well , lower the temperature to -25°C, add 2000g (8.05mol, 1.2equiv) of iodine in equal amounts in batches, and react at -10°C for 3h after feeding is complete;
[0045] 2) Add 900 mL (15.74 mol) of acetic acid and 700 g (3.11 mol) of N-iodosuccinimide in batches to the reaction solution in step 1), and react at -10°C for 1 h;
[0046] 3) Mix and stir 2000g (15.87mol) of sodium sulfite, 1100g (10.38mol) of sodium carbonate and 20L of water evenly, cool down to 5°C to obtain an alkali solution, and slowly add the alkali solution dropwise to the reaction solution in step 2) After the addition, adjust the pH of the system to 9 with saturated sodium carbonate solution, stir for 2 hours, filter, and the filtered solid is beaten with ...
Embodiment 3
[0048] A preparation method of 4-amino-7-iodopyrrolo[2,1-f][1,2,4]triazine, comprising the following steps:
[0049] 1) Under nitrogen protection, add 80g (0.6mol) of 4-aminopyrrolo[2,1-f][1,2,4]triazine into 400mL of N,N-dimethylformamide and stir well , lower the temperature to -25°C, add 181.8g (0.716mol, 1.2equiv) of iodine in equal amounts in batches, and react at -10°C for 3h after feeding is complete;
[0050] 2) Add 80 mL (1.35 mol) of formic acid and 60 g (0.24 mol, 0.4 equiv) of N-iodosuccinimide in batches to the reaction solution in step 1), and react at -10°C for 1 h;
[0051] 3) Mix and stir 225.7g (1.791mol, 3equiv) of sodium sulfite, 101.2g (0.955mol, 1.6equiv) of sodium carbonate and 2000mL of water evenly, cool down to 5°C to obtain an alkali solution, and slowly add the alkali solution dropwise Into the reaction solution of step 2), adjust the pH of the system to 9 with saturated sodium carbonate solution after adding, stir for 2 hours, filter, the filtered...
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