4-Ethylphenylhydrazine hydrochloride synthesis
- Product Name:4-Ethylphenylhydrazine hydrochloride
- CAS Number:53661-18-0
- Molecular formula:C8H13ClN2
- Molecular Weight:172.66
589-16-2
53661-18-0
The general procedure for the synthesis of 4-ethylphenylhydrazine hydrochloride from 4-ethylaniline is as follows: 150 mL of deionized water and 160 mL of 12 N hydrochloric acid were added to a reaction flask containing 24.2 g (0.2 mol) of 4-ethylaniline. After cooling the reaction mixture to 0°C, 14 g (0.2 mol) of sodium nitrite solution dissolved in 140 mL of water was added slowly and dropwise. The reaction temperature was maintained at 0 °C and after 1 h, 112 g (0.496 mol) of stannous chloride dihydrate solution pre-dissolved in 90 mL of 12 N hydrochloric acid was added to the reaction mixture, controlling the temperature of the reaction not to exceed 10 °C during the addition process. After the addition, the reaction was continued with stirring at 10 °C for 1.5 h. The reaction mixture was cooled to 0 °C and then filtered. Upon completion of the reaction, the reaction mixture was filtered and the brown solid product was collected with a measured melting point of 198°C and 95% yield.
589-16-2
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53661-18-0
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Yield: 95%
Reaction Conditions:
Stage #1:4-aminoethylbenzene with hydrogenchloride;sodium nitrite in water at 0; for 1 h;
Stage #2: with hydrogenchloride;tin(ll) chloride in water at -10; for 1.5 h;
Steps:
B.3.1 Preparation of 5-ethyl-1H-2-indolecarboxylic Acid (According to the Fischer Method)-(Compound B.3); 3rd Method:; Step 1: 4-Ethylphenylhydrazine Hydrochloride.
150 ml of water and 160 ml of 12N hydrochloric acid are added to 24.2 g (0.2 mol) of 4-ethylaniline. The mixture is cooled to 0 C. and 14 g (0.2 mol) of sodium nitrite dissolved in 140 ml of water are then introduced dropwise. After 1 hour at 0 C., 112 g (0.496 mol) of stannous chloride dihydrate dissolved in 90 ml of 12 N hydrochloric acid are added to the reaction mixture, at 10 C. After 1 hour 30 at 10 C., the reaction mixture is ltered in order to obtain a brown solid, m.p.=198 C.; yield=95%.
References:
Bignon, Eric;Bras, Jean Pierre;De Cointet, Paul;Despeyroux, Pierre;Frehel, Daniel;Gully, Danielle US2004/43995, 2004, A1 Location in patent:Page 13
1585-07-5
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53661-18-0
149 suppliers
$7.00/250mg
25309-64-2
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53661-18-0
149 suppliers
$7.00/250mg