N,1,3-TRIMETHYL-1H-PYRAZOL-5-AMINE synthesis
- Product Name:N,1,3-TRIMETHYL-1H-PYRAZOL-5-AMINE
- CAS Number:103068-68-4
- Molecular formula:C6H11N3
- Molecular Weight:125.17
1590502-62-7
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103068-68-4
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Yield:103068-68-4 70%
Reaction Conditions:
with potassium hydroxide in ethanol;water; for 10 h;Reflux;
Steps:
3.4. Preparation of N,1,3-Trimethyl-1H-pyrazol-5-amine (15)
To a solution of N-(1,3-dimethyl-1H-pyrazol-5-yl)-N-methylacetamide (14, 7.16 g, 42 mmol) in ethanol (69 mL) was added a 5 N aqueous solution of KOH (40 mL), and the mixture was refluxed for 10 h. After this time the reaction mixture was first filtered and then evaporated under vacuum to give a residue which was extracted with diethyl ether (4 × 90 mL). The combined extracts were evaporated under reduced pressure and the obtained residue was processed by flash chromatography [13]: column external diameter 4 cm, silica gel 0.040-0.063 mm, ethyl acetate/acetone (1:1 v/v ) as eluent (1.5 L), fractions each 50 mL. The first ten fractions were discarded, and fractions 11-25 were evaporated affording pure 15 as a pale yellow oil in 70% yield. IR (KBr, cm-1): 3,228 (NH); 1H-NMR (CDCl3,ppm): 2.18 (3H, s, CH3), 2.80 (3H, s, CH3), 3.53 (4H, s, CH3, NH; 3H after exchange with D2O), 5.27(1H, s, pyrazole H-4); Anal. Calcd. for C6H11N3 (125.17) : C, 57.57%; H, 8.86%; N, 33.57%. Found:C, 57.21%; H, 8.86%; N, 33.53%.
References:
Maggio, Benedetta;Raffa, Demetrio;Raimondi, Maria Valeria;Daidone, Giuseppe [Molecules,2013,vol. 18,# 10,p. 13096 - 13110]
3524-32-1
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75092-37-4
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103068-68-4
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34605-62-4
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