PYRAZINE-2-CARBOXAMIDINE HYDROCHLORIDE synthesis
- Product Name:PYRAZINE-2-CARBOXAMIDINE HYDROCHLORIDE
- CAS Number:138588-41-7
- Molecular formula:C5H7ClN4
- Molecular Weight:158.59
19847-12-2
347 suppliers
$6.00/5g
138588-41-7
95 suppliers
$13.00/1g
Yield: 95%
Reaction Conditions:
Stage #1:2-pyrazine carbonitrile with sodium methylate in methanol at 20 - 30; for 6 h;
Stage #2: with ammonium chloride at 25; for 22 h;
Steps:
1; 1.a Pyrazine-2-carboxamidine hydrochloride
To a solution of sodium methoxide (NaOCH3) (51.4 g, 0.952 mol) in methanol (3800 ml) there is added cyanopyrazine (1.00 KG, 9.53 mol) slowly at room temperature. The mixture is heated to 30° C. and stirred for 6 h. The mixture is cooled to 25° C. followed by the addition of ammonium chloride (NH4Cl) (572 g, 10.5 mol). The reaction mixture is stirred for 22 h and methyl t-butyl ether (4000 mL) is added and the mixture is stirred for 15 min forming a solid. The solid is filtered and washed with methyl t-butyl ether (2×1000 mL) then dried at 40° C./0-10 mmHg for 17 h to give white solid product (1435 g) in 95% yield with 95% HPLC purity. 1H NMR (DMSO-D6): δ 9.7 (bs, 3H), 9.49 (d, 1H, J=1.5 Hz), 9.04 (m, 1H), 8.93 (t, 1H, J=1.5 Hz)
References:
Wyeth US2006/281760, 2006, A1 Location in patent:Page/Page column 5; 8
67-56-1
757 suppliers
$7.29/5ml-f
19847-12-2
347 suppliers
$6.00/5g
138588-41-7
95 suppliers
$13.00/1g