ChemicalBook CAS DataBase List PYRROLO[1,2-F][1,2,4]TRIAZIN-4-AMINE

PYRROLO[1,2-F][1,2,4]TRIAZIN-4-AMINE synthesis

10synthesis methods

Product Name:PYRROLO[1,2-F][1,2,4]TRIAZIN-4-AMINE
CAS Number:159326-68-8
Molecular formula:C6H6N4
Molecular Weight:134.14

109-97-7 Synthesis

109-97-7
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1189-71-5
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$18.00/5g

3473-63-0 Synthesis

3473-63-0
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159326-68-8
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$10.00/250mg

Yield:159326-68-8 1358.6 g

Reaction Conditions:

Stage #1: pyrrole;isocyanate de chlorosulfonyle in N,N-dimethyl-formamide;acetonitrile at 5; for 2.5 h;Large scale;
Stage #2: with O-[4-nitro-2-(trifluoromethyl)phenyl]hydroxylamine in N,N-dimethyl-formamide;acetonitrile at 40 - 80; for 4 h;Large scale;
Stage #3: formamidine acetic acidwith potassium carbonate in N,N-dimethyl-formamide;acetonitrile at 70 - 80; for 5 h;Large scale;Temperature;

Steps:

1-5 Example 3

Add 40L of acetonitrile, 1000g (14.9mol, 1.0eq) of pyrrole, 4218g (29.8mol, 2eq) of chlorosulfonic acid isocyanate into a 100L reactor, stir to dissolve, after dissolution, cool down, when the temperature of the reaction system is 5,Begin to slowly add 1LN,N-dimethylformamide dropwise, keep the temperature for 2.5h,After the incubation, the temperature was raised to 40°C, 4962g (22.4mol, 1.5eq) of O-[4-nitro-2-(trifluoromethyl)phenyl]hydroxylamine was added to the reaction solution, and then the temperature was raised to 80°C , The incubation reaction 4h,After the incubation, add 6198g (59.6mol, 4eq) formamidine acetate and 10kg (74.5mol, 5eq) of potassium carbonate to the system, maintain the temperature at 70 to 80, and keep it for 5h.After keeping warm,Slowly add 10L of water to the reaction system, then concentrate the reaction solution until no liquid drips out, cool to 10°C, stir and crystallize for 5h, wash the filter cake with 10L water, and recrystallize the filter cake with 15L ethyl acetate.Filter and dry the cake, vacuum dry at 451358.6 g of light yellow solid pyrrolo[2,1-F][1,2,4]triazine-4-amine was obtained.

References:

CN111533747,2020,A Location in patent:Paragraph 0030-0031; 0038-0039; 0043-0044; 0048-0049; 0053

3473-63-0 Synthesis

3473-63-0
486 suppliers
$5.00/25g