2-(2-methoxyphenyl)-5-methyl-2H-pyrazol-3-ylamine synthesis
- Product Name:2-(2-methoxyphenyl)-5-methyl-2H-pyrazol-3-ylamine
- CAS Number:91331-85-0
- Molecular formula:C11H13N3O
- Molecular Weight:203.24
1118-61-2
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$9.00/25g
6971-45-5
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$9.00/1g
91331-85-0
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$457.00/1g
Yield:91331-85-0 95%
Reaction Conditions:
Stage #1: 3-Aminocrotononitrile;2-methoxyphenylhydrazine hydrochloridewith hydrogenchloride in water at 100; for 18 h;
Stage #2: with sodium hydroxide in water; pH=> 12;
Steps:
51A
2.000 g (11.453 mmol) of 2-methoxyphenylhydrazine hydrochloride was put in 10 ml of IN hydrochloric acid and 0.997 g (12.140 mmol) of 3-aminocrotonic nitrile was added. The mixture was stirred for 18 h at 1000C. After cooling, the pH value of the mixture was adjusted with IN sodium hydroxide solution to pH > 12. It was extracted with dichloromethane three times. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried over sodium sulfate and concentrated in a rotary evaporator at reduced pressure. The product was dried under high vacuum. We obtained 2.430 g (purity according to LC-MS 91%, 95% of theor.) of the target compound.LC-MS (method 3): R, = 0.31 min; MS (EIpos): m/z = 204 [M+H]+.
References:
WO2010/20363,2010,A1 Location in patent:Page/Page column 89
