ethyl 2,2-dimethylpropanoate

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a refluxed solution of sodium hydride (33.18 g, 553.03 mmol) in 275 mL of cyclohexane is added a mixture of 2,2-dimethyl-propionic acid ethyl ester (30 g, 230.43 mmol) in 79 mL acetonitrile (553.03 mmol) in 25 mL of cyclohexane. The mixture is maintained at 80° C. overnight. The mixture is cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined organics are washed with water, dried over sodium sulfate, filtered and concentrated to afford title compound which was used crude in subsequent reaction. ESI m/z 124=MH− The mixture is cooled to room temperature extracted with ethyl acetate The combined organics are washed with water dried over sodium sulfate filtered concentrated

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

実験手順: Using analogous procedures to those described in the portion of Note [36] immediately above that is concerned with the preparation of starting materials, ethyl pivaloate was reacted with acetonitrile to give 4,4-dimethyl-3-oxopentanenitrile which in turn was reacted with hydrazine hydrate to give the required starting material.

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

実験手順: Absolute ethanol (1035 ml) was added to 306 grams of neopentanoic acid (Exxon) in a flask fitted with a heating mantle and a reflux condenser. To this mixture was slowly added 65 ml of concentrated sulfuric acid (Mallinckrodt). The mixture was then heated under reflux for three hours. Heating was discontinued and the hot mixture was extracted with 4 liters of a 10% sodium carbonate solution. The organic layer which separated was collected and dried overnight with magnesium sulfate. It was then filtered and purified by distillation at atmospheric pressure. A low heat was first applied in order to collect a fraction at a temperature of 73° C. consisting principally of ethanol. When the head temperature began to drop, the heat was raised and a second fraction, consisting of ethyl pivalate was collected from 108°-111° C. This pure ethyl pivalate (yield about 77%) was then dried over magnesium sulfate. fitted with a heating mantle and a reflux condenser The mixture was then heated under reflux for three hours Heating the hot mixture was extracted with 4 liters of a 10% sodium carbonate solution The organic layer which separated was collected dried overnight with magnesium sulfate It was then filtered purified by distillation at atmospheric pressure A low heat to collect a fraction at a temperature of 73° C. the heat was raised was collected from 108°-111° C

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a refluxed solution of sodium hydride (33.18 g, 553.03 mmol) in 275 mL of cyclohexane is added a mixture of 2,2-dimethyl-propionic acid ethyl ester (30 g, 230.43 mmol) in 79 mL acetonitrile (553.03 mmol) in 25 mL of cyclohexane. The mixture is maintained at 80° C. overnight. The mixture is cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined organics are washed with water, dried over sodium sulfate, filtered and concentrated to afford title compound which was used crude in subsequent reaction. ESI m/z 124=MH− The mixture is cooled to room temperature extracted with ethyl acetate The combined organics are washed with water dried over sodium sulfate filtered concentrated