Benzenamine, 2-ethyl-4-nitro- synthesis
- Product Name:Benzenamine, 2-ethyl-4-nitro-
- CAS Number:6853-29-8
- Molecular formula:C8H10N2O2
- Molecular Weight:166.18
578-54-1
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Yield:6853-29-8 96.6%
Reaction Conditions:
Stage #1: ortho-ethylanilinewith sulfuric acid at 0; for 0.333333 h;
Stage #2: with HNO3 at 33; for 15 h;Temperature;
Steps:
1.1; 2.1; 3.1 A synthetic method of 2-ethyl-1-fluoro-4-nitrobenzene, the synthetic method comprises the steps:
(1) 160g of concentrated sulfuric acid was added to the reactor, cooled to 0°C, 20g of compound A was added,Stir for 20min, then add 80g of 65% nitric acid solution, keep warm for 1h, rise to 33°C, stir for 15h, get TLC detection, the reaction of raw materials is completed, pour the reaction solution into ice water, adjust pH with 20% sodium hydroxide aqueous solution To 8-9, add 800 mL of ethyl acetate, filter through celite, separate the layers, extract the aqueous phase with ethyl acetate (400 mL), combine the organic phases, mix the silica gel samples and pass through the column, mobile phase: n-hexane/ethyl acetate= 5/1, the target product was collected and concentrated to obtain 26.5% of yellow solid to obtain compound B with a yield of 96.6%;
References:
CN114507143,2022,A Location in patent:Paragraph 0005; 0010; 0012; 0014
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