1,4,8-triazacycloundecane

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:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3.62 g of 1,4,8-triazacycloundecane and 3.75 g of hexamethylphosphorous triamide is heated to 125° C. with stirring and held at this temperature for 2 hours, by which time evolution of dimethylamine is complete. Evolution is vigorous for the first 45 minutes. Distillation affords 3.20 g (75%) 1,4,8-triaza-12-phosphatricyclo[6.3.1.04,12 ]dodecane as a water-white liquid which boils at 73°-75° C. at 0.30 mm. is vigorous for the first 45 minutes Distillation

反応条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3.62 g of 1,4,8-triazacycloundecane and 3.75 g of hexamethylphosphorous triamide is heated to 125° C. with stirring and held at this temperature for 2 hours, by which time evolution of dimethylamine is complete. Evolution is vigorous for the first 45 minutes. Distillation affords 3.20 g (75%) 1,4,8-triaza-12-phosphatricyclo[6.3.1.04,12 ]dodecane as a water-white liquid which boils at 73°-75° C. at 0.30 mm. is vigorous for the first 45 minutes Distillation

反応条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3.62 g of 1,4,8-triazacycloundecane and 3.75 g of hexamethylphosphorous triamide is heated to 125° C. with stirring and held at this temperature for 2 hours, by which time evolution of dimethylamine is complete. Evolution is vigorous for the first 45 minutes. Distillation affords 3.20 g (75%) 1,4,8-triaza-12-phosphatricyclo[6.3.1.04,12 ]dodecane as a water-white liquid which boils at 73°-75° C. at 0.30 mm. is vigorous for the first 45 minutes Distillation

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

実験手順: In a manner similar to that of Example 1 (C), 5.28 g (33.6 mmol) of 1,4,8-triazacycloundecane and 4.00 g of dimethylformamide dimethyl acetal were reacted to give 4.59 g of 1,4,8-triazatricyclo[6.3.1.04,12 ]dodecane as a clear, colorless liquid, bp 80°-82° (three fractions) (1.2 mm), nD24 = 1.5182. A fraction boiling at 82° was analyzed.

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: In a manner similar to that of Example 1 (C), 5.28 g (33.6 mmol) of 1,4,8-triazacycloundecane and 4.00 g of dimethylformamide dimethyl acetal were reacted to give 4.59 g of 1,4,8-triazatricyclo[6.3.1.04,12 ]dodecane as a clear, colorless liquid, bp 80°-82° (three fractions) (1.2 mm), nD24 = 1.5182. A fraction boiling at 82° was analyzed.

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

実験手順: In a manner similar to that of Example 1 (C), 5.28 g (33.6 mmol) of 1,4,8-triazacycloundecane and 4.00 g of dimethylformamide dimethyl acetal were reacted to give 4.59 g of 1,4,8-triazatricyclo[6.3.1.04,12 ]dodecane as a clear, colorless liquid, bp 80°-82° (three fractions) (1.2 mm), nD24 = 1.5182. A fraction boiling at 82° was analyzed.

反応条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3.62 g of 1,4,8-triazacycloundecane and 3.75 g of hexamethylphosphorous triamide is heated to 125° C with stirring and held at this temperature for 2 hours, by which time evolution of dimethylamine is complete. Evolution is vigorous for the first 45 minutes. Distillation affords 3.20 g (75%) 1,4,8-triaza-12-phosphatricyclo-[6.3.1.04,12 ]dodecane as a water-white liquid which boils at 73°-75° C at 0.30 mm. is vigorous for the first 45 minutes Distillation

反応条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 3.62 g of 1,4,8-triazacycloundecane and 3.75 g of hexamethylphosphorous triamide is heated to 125° C. with stirring and held at this temperature for 2 hours, by which time evolution of dimethylamine is complete. Evolution is vigorous for the first 45 minutes. Distillation affords 3.20 g (75%) 1,4,8-triaza-12-phosphatricyclo[6.3.1.04,12 ]dodecane as a water-white liquid which boils at 73°-75° C. at 0.30 mm. is vigorous for the first 45 minutes Distillation

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

実験手順: In a manner similar to that of Example 1 (C), 5.28 g (33.6 mmol) of 1,4,8-triazacycloundecane and 4.00 g of dimethylformamide dimethyl acetal were reacted to give 4.59 g of 1,4,8-triazatricyclo[6.3.1.04,12 ]dodecane as a clear, colorless liquid, bp 80°-82° (three fractions) (1.2 mm), nD24 = 1.5182. A fraction boiling at 82° was analyzed.