2-甲氧基丙腈

反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 2 liter stirred autoclave was placed 60 g of Raney nickel 2400 and 120 g of anhydrous ammonia. A heel of 200 g of methanol was then pumped into the reactor and the reactor externally heated to 90° C. The pressure was raised to 850 psig with hydrogen. The crude product mixture of methoxypropionitrile (MOPN) and bis(cyanoethoxy)ethane from Example 4 was then pumped into the autoclave at a rate of 5.0 g/min until 999 g of the mixture had been admitted. During the addition the temperature was maintained at 90° C. and the pressure at 850 psig with hydrogen. Following the addition, hydrogen uptake ceased within 30 min. and the reaction was terminated. The contents of the autoclave were cooled and then filtered through Celite™ filtration aid. The filtrate was analyzed by GC and found to be comprised of 16.8 wt % 3-methoxypropylamine (MOPA), 77.0 wt % of bis(3-aminopropoxy)ethane, 0.89 wt % of 3-aminopropoxyethanol, 1.96 wt % of N-methoxypropyl-bis(3-amino-propoxy)ethane, 0.35 wt % of bis(3-methoxypropyl)amine and 3.0 wt % of bis(aminopropoxyethoxypropyl)amine. During the addition the temperature was maintained at 90° C. the reaction was terminated The contents of the autoclave were cooled filtered through Celite™ filtration aid

反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 2 liter stirred autoclave was placed 60 g of Raney nickel 2400 and 120 g of anhydrous ammonia. A heel of 200 g of methanol was then pumped into the reactor and the reactor externally heated to 90° C. The pressure was raised to 850 psig with hydrogen. The crude product mixture of methoxypropionitrile (MOPN) and bis(cyanoethoxy)ethane from Example 4 was then pumped into the autoclave at a rate of 5.0 g/min until 999 g of the mixture had been admitted. During the addition the temperature was maintained at 90° C. and the pressure at 850 psig with hydrogen. Following the addition, hydrogen uptake ceased within 30 min. and the reaction was terminated. The contents of the autoclave were cooled and then filtered through Celite™ filtration aid. The filtrate was analyzed by GC and found to be comprised of 16.8 wt % 3-methoxypropylamine (MOPA), 77.0 wt % of bis(3-aminopropoxy)ethane, 0.89 wt % of 3-aminopropoxyethanol, 1.96 wt % of N-methoxypropyl-bis(3-amino-propoxy)ethane, 0.35 wt % of bis(3-methoxypropyl)amine and 3.0 wt % of bis(aminopropoxyethoxypropyl)amine. During the addition the temperature was maintained at 90° C. the reaction was terminated The contents of the autoclave were cooled filtered through Celite™ filtration aid

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: As in Example 1, bis(2-cyanoethoxy)ethane was prepared by the addition of 623 g (11.73 moles) of acrylonitrile to 310 g (5.0 moles) of ethylene glycol containing 1.0 g of anhydrous lithium hydroxide at 55°-60° C. over a period of 90 min. The reaction was permitted to stir an additional 2 hr at 50° C. The reaction contents were cooled to 25° C. and 88.0 g (2.75 moles) of methanol was added over a period of 1 hr while maintaining the temperature between 25°-30° C. The mixture was allowed to stir an additional 12 hr at room temperature. Analysis by NMR revealed the crude product mixture to be 79.7 wt % of bis(2-cyanoethoxy)ethane, 17.4 wt % methoxypropionitrile, 1.78 wt % methanol, 0.72 wt % of 2-cyanoethoxyethanol, and 0.33 wt % acrylonitrile. The reaction contents were cooled to 25° C. while maintaining the temperature between 25°-30° C to stir an additional 12 hr at room temperature

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.8 g. of sodium were dissolved in 120 ml. of methanol under reflux. 56 g. of methoxypropionitrile and 60 g. of 3-methoxy-4,5-methylenedioxybenzaldehyde were then added and refluxed in the methanol mixture for 5 hours. Upon chilling, 3-methoxy-4,5-methylenedioxy-α-methoxymethyl-cinnamonitrile crystallized in needles of m.p. = 115°, in a yield of 68 g.= 83 percent. A sample for analysis was recrystallized from methanol, m.p. 115.5°-116.5°. Upon chilling 3-methoxy-4,5-methylenedioxy-α-methoxymethyl-cinnamonitrile crystallized in needles of m.p. = 115°, in a yield of 68 g A sample for analysis was recrystallized from methanol, m.p. 115.5°-116.5°

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.8 g. of sodium were dissolved in 120 ml. of methanol under reflux. 56 g. of methoxypropionitrile and 60 g. of 3-methoxy-4,5-methylenedioxybenzaldehyde were then added and refluxed in the methanol mixture for 5 hours. Upon chilling, 3-methoxy-4,5-methylenedioxy-α-methoxymethyl-cinnamonitrile crystallized in needles of m.p. = 115°, in a yield of 68 g. = 83 percent. A sample of analysis was recrystallized from methanol, m.p. 115.5°-116.5°. Upon chilling 3-methoxy-4,5-methylenedioxy-α-methoxymethyl-cinnamonitrile crystallized in needles of m.p. = 115°, in a yield of 68 g A sample of analysis was recrystallized from methanol, m.p. 115.5°-116.5°

反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 2 liter stirred autoclave was placed 60 g of Raney nickel 2400 and 120 g of anhydrous ammonia. A heel of 200 g of methanol was then pumped into the reactor and the reactor externally heated to 90° C. The pressure was raised to 850 psig with hydrogen. The crude product mixture of methoxypropionitrile (MOPN) and bis(cyanoethoxy)ethane from Example 4 was then pumped into the autoclave at a rate of 5.0 g/min until 999 g of the mixture had been admitted. During the addition the temperature was maintained at 90° C. and the pressure at 850 psig with hydrogen. Following the addition, hydrogen uptake ceased within 30 min. and the reaction was terminated. The contents of the autoclave were cooled and then filtered through Celite™ filtration aid. The filtrate was analyzed by GC and found to be comprised of 16.8 wt % 3-methoxypropylamine (MOPA), 77.0 wt % of bis(3-aminopropoxy)ethane, 0.89 wt % of 3-aminopropoxyethanol, 1.96 wt % of N-methoxypropyl-bis(3-amino-propoxy)ethane, 0.35 wt % of bis(3-methoxypropyl)amine and 3.0 wt % of bis(aminopropoxyethoxypropyl)amine. During the addition the temperature was maintained at 90° C. the reaction was terminated The contents of the autoclave were cooled filtered through Celite™ filtration aid

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: As in Example 1, bis(2-cyanoethoxy)ethane was prepared by the addition of 623 g (11.73 moles) of acrylonitrile to 310 g (5.0 moles) of ethylene glycol containing 1.0 g of anhydrous lithium hydroxide at 55°-60° C. over a period of 90 min. The reaction was permitted to stir an additional 2 hr at 50° C. The reaction contents were cooled to 25° C. and 88.0 g (2.75 moles) of methanol was added over a period of 1 hr while maintaining the temperature between 25°-30° C. The mixture was allowed to stir an additional 12 hr at room temperature. Analysis by NMR revealed the crude product mixture to be 79.7 wt % of bis(2-cyanoethoxy)ethane, 17.4 wt % methoxypropionitrile, 1.78 wt % methanol, 0.72 wt % of 2-cyanoethoxyethanol, and 0.33 wt % acrylonitrile. The reaction contents were cooled to 25° C. while maintaining the temperature between 25°-30° C to stir an additional 12 hr at room temperature