1,1,1,2-tetrachloroethane

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反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: 1 mole of 2-acetamido-5-bromothiophen was reacted with 1 mole dimethylformamide and 3 moles phosphorus oxychloride under reflux in tetrachloroethane for 3 hours at a temperature of 138° C. The compound of formula V in which R1 represents bromo, X represents chloro, and R2, R3 and R4 represent hydrogen was isolated in a yield of 66%. The remainder of the product was accounted for, mainly as unreacted starting material together with a small amount (ca 1%) of polymeric materials. The specified compound of formula V (2-bromo-6-chloro-thieno{2,3-b}-pyridine) was isolated from the crude product by chromatography on a short column of alumina using light petroleum spirit as eluant. The compound was recrystallised from ethanol and had a melting point of 116° C. was isolated in a yield of 66%

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反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 1 L three-necked, round-bottomed flask equipped with a magnetic stirrer, thermometer, condenser, and a nitrogen atmosphere are charged 20.0 g (61.9 mmol) of 2-chloro-4,6-bis-(2,4-dimethylphenyl)-s-triazine and 50 mL of tetrachloroethane. The mixture is warmed to dissolve the solids and 8.24 g (62.0 mmol) of aluminum chloride are added in small portions all at once followed by 9.00 g (62.1 mmol) of 4-chlororesorcinol. The mixture is stirred at 120° C. for four hours. After cooling to room temperature 50 mL of water and 10 mL of concentrated hydrochloric acid are added and the mixture is refluxed for two hours. After cooling, the mixture is extracted thrice with ethyl acetate and the combined organic layers are dried over anhydrous magnesium sulfate and filtered. The solvent is removed under reduced pressure to yield a yellow solid. Recrystallization from ethyl acetate/heptane affords 8.65 g of the title compound as a yellow solid. To a 1 L three-necked, round-bottomed flask equipped with a magnetic stirrer The mixture is warmed are added in small portions are added the mixture is refluxed for two hours After cooling the mixture is extracted thrice with ethyl acetate the combined organic layers are dried over anhydrous magnesium sulfate filtered The solvent is removed under reduced pressure to yield a yellow solid Recrystallization from ethyl acetate/heptane