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ChemicalBook CAS DataBase List Thiophene-2-ethylamine

Thiophene-2-ethylamine synthesis

7synthesis methods
N,N-Dimethylformamide (DMF) reacts with thiophene to obtain 2-thiophenecarbaldehyde, then reacts with isopropyl chloroacetate to obtain 2-thiopheneacetaldehyde, and then reacts with hydroxylamine hydrochloride to obtain 2-thiopheneacetaldehyde oxime, and finally reduced to give 2-thiopheneethylamine.
-

Yield:30433-91-1 1009 g

Reaction Conditions:

with hydrogen at 120; for 12 h;Autoclave;

Steps:

1 Path B
The 10M2-chlorothiophene and 10M metal magnesium reagent format preparation, cooled to room temperature,Add 1000ml of anhydrous tetrahydrofuran, mix well,Slowly add 10M (the material optional range of 8-10M) nitroethylene,The reaction was refluxed for 3 hours (depending on the different substituted thiophene anion derivative,The reaction time is 3-12 hours, such as:The reaction time for the substitution of electron groups on the ring is 3-8 hours,The ring has a substitution of electron-withdrawing groups when the reaction time is 8-12 hours), the solvent was removed under reduced pressure stand-by.The above product was dissolved in 3000 ml of DMSO, 10M acetic acid was added dropwise and reacted at 120 ° C for 5 hours,Recrystallization gave 1231 g of product.Or the product was added 1MPd / C or Raney Ni, 10M of hydrogen was introduced in an autoclave, at120 ° C for 12 hours, filtered, extracted, and distilled under reduced pressure to obtain the product 1009g.

References:

Wang Zhixun CN106554343, 2017, A Location in patent:Paragraph 0039; 0040; 0041

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