反应详情

A stirred solution of 5.00 g of 2-amino-N-methyl-α-(3-methyl-2-thienyl)benzeneethanamine and 235 ml of ethyl formate was refluxed for 8 hours. Volatile components were removed at 60° C. on a rotary evaporator. Thin layer chromatography (silica gel, ethyl acetate as the eluent) of the resultant oil indicated a multi-component mixture. HPLC of the mixture (Water's Associates Prep LC/System 500, silica gel, elution with ethyl acetate) permitted component separation. The faster eluting fractions were concentrated to an oil which crystallized upon standing. Recrystallization from methanol-water afforded 1.2 g of 2-amino-N-formyl-N-methyl-α-(3-methyl-2-thienyl)benzeneethanamine, mp 111°-112° C.

1. customVolatile components were removed at 60° C. on a rotary evaporator
2. washHPLC of the mixture (Water's Associates Prep LC/System 500, silica gel, elution with ethyl acetate)
3. customcomponent separation
4. washThe faster eluting fractions
5. concentrationwere concentrated to an oil which
6. customcrystallized
7. customRecrystallization from methanol-water