ChemicalBook CAS DataBase List 1-Methyl-5-nitro-1H-benzotriazole

1-Methyl-5-nitro-1H-benzotriazole synthesis

4synthesis methods

Product Name:1-Methyl-5-nitro-1H-benzotriazole
CAS Number:25877-34-3
Molecular formula:C7H6N4O2
Molecular Weight:178.15

41939-61-1 Synthesis

41939-61-1
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25877-34-3
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Yield:25877-34-3 81%

Reaction Conditions:

Stage #1: N₁-methyl-4-nitrobenzene-1,2-diaminewith hydrogenchloride;sodium nitrite in water at 0; for 3 h;
Stage #2: with potassium hydroxide in water;

Steps:

55; 142.1

A stirred suspension of diamine 248 (1.13g, 6. 76mmol) and concentrated HCI (5.6 mL, 67 mmol) in water (22 mL) at ODC, was treated with a solution of NaNO2 (586 mg, 8.5 mmol) in water (10 mL). The mixture was stirred at the same conditions for 3h, warmed to room temperature, neutralized with a 5% w/v solution of KOH in water and filtered. The solid was washed with cold water and dried to afford title compound 264 (975mg, 81% yields NMR: (DMSO) 8 (ppm): 9.00 (d, J = 1.3 Hz, 1H), 8.39 (dd, J = 1.3, 8.8 Hz, 1H), 8.09 (d, J = 8.8 Hz, lH), 4. 40 (s, 3H).

References:

WO2005/92899,2005,A1 Location in patent:Page/Page column 155