tert-butyl 1-chloroethyl carbonate

反応条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: t-Butanol (3.34 mL, 35 mmol) and pyridine (3.39 mL, 42 mmol) were dissolved in 90 mL methylene chloride and cooled to −78° C. 1-Chloroethyl chloroformate (5.0 g, 35 mmol) was added dropwise and the reaction was slowly allowed to warm to room temperature, then stirred for 3 days. The r×n was evaporated, dissolved in ethyl acetate, then washed with water and brine, dried over magnesium sulfate and evaporated. It was noted that product evaporated under high vacuum. The product was distilled to yield 1-chloroethyl t-butyl carbonate a colorless oil (2.46 g, 39% yield).). 1H NMR (400 MHz, CDCl3) δ 6.41 (d, J=5.6 Hz, 1H), 1.82 (d, J=5.6 Hz, 3H), 1.53 (s, 9H). to warm to room temperature The r×n was evaporated dissolved in ethyl acetate washed with water and brine dried over magnesium sulfate evaporated evaporated under high vacuum The product was distilled

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

実験手順: The procedure is as in Example 7, but with 8.5 g (0.1 mole) of piperidine, 60 ml of THF, 20 ml of saturated aqueous K2CO3 solution and 0.11 mole of α-chloroethyl tert-butyl carbonate.

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

実験手順: In a reactor cooled to +5° C., there are introduced 600 ml of dicloromethane, 43.7 g (0.59 mole) of tert-butanol and 94.7 g (0.66 mole) of α-chloroethyl chloroformate. 57 g (0.72 mole) of pyridine are then added dropwise and with stirring while the temperature is maintained at between 10° and 20° C. The mixture is stirred for 4 hours at room temperature. In a reactor cooled to +5° C. is maintained at between 10° and 20° C The mixture is stirred for 4 hours at room temperature

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

実験手順: The procedure is as in Example 7, but with 8.5 g (0.1 mole) of piperidine, 60 ml of THF, 20 ml of saturated aqueous K2CO3 solution and 0.11 mole of α-chloroethyl tert-butyl carbonate.

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

実験手順: In a reactor cooled to +5° C., there are introduced 600 ml of dicloromethane, 43.7 g (0.59 mole) of tert-butanol and 94.7 g (0.66 mole) of α-chloroethyl chloroformate. 57 g (0.72 mole) of pyridine are then added dropwise and with stirring while the temperature is maintained at between 10° and 20° C. The mixture is stirred for 4 hours at room temperature. In a reactor cooled to +5° C. is maintained at between 10° and 20° C The mixture is stirred for 4 hours at room temperature

反応条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: t-Butanol (3.34 mL, 35 mmol) and pyridine (3.39 mL, 42 mmol) were dissolved in 90 mL methylene chloride and cooled to −78° C. 1-Chloroethyl chloroformate (5.0 g, 35 mmol) was added dropwise and the reaction was slowly allowed to warm to room temperature, then stirred for 3 days. The r×n was evaporated, dissolved in ethyl acetate, then washed with water and brine, dried over magnesium sulfate and evaporated. It was noted that product evaporated under high vacuum. The product was distilled to yield 1-chloroethyl t-butyl carbonate a colorless oil (2.46 g, 39% yield).). 1H NMR (400 MHz, CDCl3) δ 6.41 (d, J=5.6 Hz, 1H), 1.82 (d, J=5.6 Hz, 3H), 1.53 (s, 9H). to warm to room temperature The r×n was evaporated dissolved in ethyl acetate washed with water and brine dried over magnesium sulfate evaporated evaporated under high vacuum The product was distilled

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

実験手順: The procedure is as in Example 7, but with 8.5 g (0.1 mole) of piperidine, 60 ml of THF, 20 ml of saturated aqueous K2CO3 solution and 0.11 mole of α-chloroethyl tert-butyl carbonate.

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

実験手順: In a reactor cooled to +5° C., there are introduced 600 ml of dicloromethane, 43.7 g (0.59 mole) of tert-butanol and 94.7 g (0.66 mole) of α-chloroethyl chloroformate. 57 g (0.72 mole) of pyridine are then added dropwise and with stirring while the temperature is maintained at between 10° and 20° C. The mixture is stirred for 4 hours at room temperature. In a reactor cooled to +5° C. is maintained at between 10° and 20° C The mixture is stirred for 4 hours at room temperature