3,5-DICHLORO-4-HYDROXYBENZOHYDRAZIDE synthesis
- Product Name:3,5-DICHLORO-4-HYDROXYBENZOHYDRAZIDE
- CAS Number:23964-29-6
- Molecular formula:C7H6Cl2N2O2
- Molecular Weight:221.04
3337-59-5
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Yield:23964-29-6 100%
Reaction Conditions:
with hydrazine in methanol; for 3 h;Heating / reflux;
Steps:
2
3,5-dichloro-4- hydroxybenzoic acid methyl ester (500 mg, 2.27 mmol) was dissolved in MeOH (15 mL). NH2NH2-H2O (5 mL) was added and the mixture was refluxed for 3 h. large amount of white solid was formed. After the reaction was completed (TLC), solvent and excess of hydrazine monohydrate were evaporated to dryness in vacuum. The crude product was obtained as a white solid (quantitative yield) and it was pure enough by NMR 1H to be used without further purification. 1H NMR (DMSO) δ: 6.50 (brs, 4H), 7.61 (s, 2H). 13C NMR (DMSO) δ: 112.91, 122.83, 126.76, 162.78, 165.52. MS m/z 221.0 (MH+, 100), 188.9 (M-NH-NH2, 96).
References:
WO2006/136008,2006,A1 Location in patent:Page/Page column 34
17302-82-8
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