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ChemicalBook CAS DataBase List 2-Ethylaminothiophene

2-Ethylaminothiophene synthesis

2synthesis methods
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Yield:203730-54-5 4.5 g

Reaction Conditions:

Stage #1: thiophen-2-ylamine;acetaldehyde in ethanol at 25; for 1 h;Inert atmosphere;
Stage #2: with sodium tetrahydroborate in ethanol at 20; for 1 h;

Steps:



In a flask, 8 g of crude product of intermediate 001-1,2 g of acetaldehyde and 40 mL of ethanol were placed,And the mixture was stirred at 25 ° C. for 1 hour under a nitrogen atmosphere.Here, 6 g of sodium borohydride was added,Carefully observe foaming, add 0.5 g each in 12 portions,The mixture was stirred at room temperature for 1 hour to obtain a reaction solution.The reaction solution was poured into 200 mL of water,It was extracted three times with 50 mL of ethyl acetate,The organic phase was collected. The collected organic phase was concentrated under reduced pressure,The residue was purified by column chromatography (packing agent: silica gel, developing solution: n-hexane / ethyl acetate (3/1)) to obtain 4.5 g of intermediate 002-1.

References:

JP2017/149805,2017,A Location in patent:Paragraph 0165-0166