2-bromo-1-cycloheptylethanone

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution composed of 6.57 g of bromomethyl cycloheptyl ketone, 6.24 g of (E)-3-(3-nitrophenyl)-2-propenethioamide and 100 ml of ethyl alcohol was heated to reflux for 16 hr afterwhich it was diluted with 200 ml of ice water and extracted with methylene chloride. The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 6.17 g of (E)-4-cycloheptyl-2-[2-(3-nitrophenyl)ethenyl]thiazole; m.p. 60° C. after crystallization from ethyl ether/hexane. was heated to reflux for 16 hr afterwhich it extracted with methylene chloride The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An ice cold solution of 19.0 g of cycloheptyl methyl ketone in 100 ml of methyl alcohol was treated dropwise with 7 ml of bromine. After 5 min, the ice bath was removed and the reaction mixture was allowed to warm to room temperature. The reaction mixture was then diluted with 500 ml of water and extracted with ethyl ether (3×75 ml). The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 29.9 g of bromomethyl cycloheptyl ketone as an oil. the ice bath was removed The reaction mixture was then diluted with 500 ml of water extracted with ethyl ether (3×75 ml) The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution composed of 6.57 g of bromomethyl cycloheptyl ketone, 6.24 g of (E)-3-(3-nitrophenyl)-2-propenethioamide and 100 ml of ethyl alcohol was heated to reflux for 16 hr afterwhich it was diluted with 200 ml of ice water and extracted with methylene chloride. The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 6.17 g of (E)-4-cycloheptyl-2-[2-(3-nitrophenyl)ethenyl]thiazole; m.p. 60° C. after crystallization from ethyl ether/hexane. was heated to reflux for 16 hr afterwhich it extracted with methylene chloride The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution composed of 6.57 g of bromomethyl cycloheptyl ketone, 6.24 g of (E)-3-(3-nitrophenyl)-2-propenethioamide and 100 ml of ethyl alcohol was heated to reflux for 16 hr afterwhich it was diluted with 200 ml of ice water and extracted with methylene chloride. The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 6.17 g of (E)-4-cycloheptyl-2-[2-(3-nitrophenyl)ethenyl]thiazole; m.p. 60° C. after crystallization from ethyl ether/hexane. was heated to reflux for 16 hr afterwhich it extracted with methylene chloride The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An ice cold solution of 19.0 g of cycloheptyl methyl ketone in 100 ml of methyl alcohol was treated dropwise with 7 ml of bromine. After 5 min, the ice bath was removed and the reaction mixture was allowed to warm to room temperature. The reaction mixture was then diluted with 500 ml of water and extracted with ethyl ether (3×75 ml). The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 29.9 g of bromomethyl cycloheptyl ketone as an oil. the ice bath was removed The reaction mixture was then diluted with 500 ml of water extracted with ethyl ether (3×75 ml) The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An ice cold solution of 19.0 g of cycloheptyl methyl ketone in 100 ml of methyl alcohol was treated dropwise with 7 ml of bromine. After 5 min, the ice bath was removed and the reaction mixture was allowed to warm to room temperature. The reaction mixture was then diluted with 500 ml of water and extracted with ethyl ether (3×75 ml). The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 29.9 g of bromomethyl cycloheptyl ketone as an oil. the ice bath was removed The reaction mixture was then diluted with 500 ml of water extracted with ethyl ether (3×75 ml) The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution composed of 6.57 g of bromomethyl cycloheptyl ketone, 6.24 g of (E)-3-(3-nitrophenyl)-2-propenethioamide and 100 ml of ethyl alcohol was heated to reflux for 16 hr afterwhich it was diluted with 200 ml of ice water and extracted with methylene chloride. The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 6.17 g of (E)-4-cycloheptyl-2-[2-(3-nitrophenyl)ethenyl]thiazole; m.p. 60° C. after crystallization from ethyl ether/hexane. was heated to reflux for 16 hr afterwhich it extracted with methylene chloride The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An ice cold solution of 19.0 g of cycloheptyl methyl ketone in 100 ml of methyl alcohol was treated dropwise with 7 ml of bromine. After 5 min, the ice bath was removed and the reaction mixture was allowed to warm to room temperature. The reaction mixture was then diluted with 500 ml of water and extracted with ethyl ether (3×75 ml). The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 29.9 g of bromomethyl cycloheptyl ketone as an oil. the ice bath was removed The reaction mixture was then diluted with 500 ml of water extracted with ethyl ether (3×75 ml) The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution composed of 6.57 g of bromomethyl cycloheptyl ketone, 6.24 g of (E)-3-(3-nitrophenyl)-2-propenethioamide and 100 ml of ethyl alcohol was heated to reflux for 16 hr afterwhich it was diluted with 200 ml of ice water and extracted with methylene chloride. The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 6.17 g of (E)-4-cycloheptyl-2-[2-(3-nitrophenyl)ethenyl]thiazole; m.p. 60° C. after crystallization from ethyl ether/hexane. was heated to reflux for 16 hr afterwhich it extracted with methylene chloride The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An ice cold solution of 19.0 g of cycloheptyl methyl ketone in 100 ml of methyl alcohol was treated dropwise with 7 ml of bromine. After 5 min, the ice bath was removed and the reaction mixture was allowed to warm to room temperature. The reaction mixture was then diluted with 500 ml of water and extracted with ethyl ether (3×75 ml). The combined extracts were washed with saturated sodium bicarbonate, brine, dried (MgSO4) and condensed in vacuo to yield 29.9 g of bromomethyl cycloheptyl ketone as an oil. the ice bath was removed The reaction mixture was then diluted with 500 ml of water extracted with ethyl ether (3×75 ml) The combined extracts were washed with saturated sodium bicarbonate, brine dried (MgSO4) and condensed in vacuo