* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Stage #1: at 20 - 80℃; for 2 h; Inert atmosphere Stage #2: Reflux
Under argon protection, 11.2 g of acetic anhydride and 25.6 g were addedN - (2-methyl-4-oxapentan-2-yl) -3-morpholinopropionamideThe raw material is mixed with 250 ml of toluene, and the temperature is slowly increased from room temperature to 60 to 80 DEG C and stirred for 2 hours. After stirringMix and then add 0.2 g inhibitor BHT and 0.1 g cuprous chloride and 10.8 g triethylamine, and gradually warmed to reflux reactionNight, the reaction system was concentrated under reduced pressure to give the crude product which was directly separated by silica gel column chromatography with hexane-ethyl acetate14.1 grams of purified pure acrylamide (85percent yield) and 9.8 grams of pure N-acetylmorpholine (76percent yield).
Reference：
[1] Patent: CN107417644, 2017, A, . Location in patent: Paragraph 0023
2
[ 67874-34-4 ]
[ 2873-97-4 ]
Reference：
[1] Patent: CN106565519, 2017, A, . Location in patent: Paragraph 0018; 0022-0027
3
[ 123-42-2 ]
[ 107-13-1 ]
[ 2873-97-4 ]
Yield
Reaction Conditions
Operation in experiment
70.4%
at 50 - 95℃; for 2.03111 - 3.27 h;
EXAMPLE 1Use of a Spiral Heat-Exchanger for the First Residence Time UnitA reaction solution with a stoichiometric molar ratio of acrylonitrile (AN) to diacetone alcohol (DiAOH) to H2SO4=1.0:1.0:2.4 had a residence time of 12 s at 90° C. in the microreactor (composed of a mixing module made from Hastelloy and of a heat-exchange module), 100 s at 90° C. in the spiral heat-exchanger, and two hours at 50° C. in the continuous stirred tank.The total yield of diacetoneacrylamide was 78percent, based on ACN, the proportions of the final conversion being 74percent in the first 12 s, 21percent in the following 100 s, and 5percent in the remaining 2 h.; EXAMPLES 2-6Execution was analogous to example 1. Table 1 shows starting materials used, residence times, temperatures, and yields:; EXAMPLE 7The reaction led to a final yield of 73.5percent, using a stoichiometric ratio of AN to DiaOH to H2SO4=1.0:1.0:2.2 and a residence time distribution, with 90° C. for 12 s in the microreactor, with 65° C. for 960 s in the first continuous stirred tank and with 55° C. for 10 800 s in the second continuous stirred tank.; EXAMPLE 8-10Execution was analogous to example 7. Table 2 shows the starting materials used, residence times, temperatures, and yields:
EXAMPLES 2-6Execution was analogous to example 1. Table 1 shows starting materials used, residence times, temperatures, and yields:; EXAMPLE 1Use of a Spiral Heat-Exchanger for the First Residence Time UnitA reaction solution with a stoichiometric molar ratio of acrylonitrile (AN) to diacetone alcohol (DiAOH) to H2SO4=1.0:1.0:2.4 had a residence time of 12 s at 90° C. in the microreactor (composed of a mixing module made from Hastelloy and of a heat-exchange module), 100 s at 90° C. in the spiral heat-exchanger, and two hours at 50° C. in the continuous stirred tank.The total yield of diacetoneacrylamide was 78percent, based on ACN, the proportions of the final conversion being 74percent in the first 12 s, 21percent in the following 100 s, and 5percent in the remaining 2 h.
poly(2-acetoacetoxyethyl methacrylate-co-diacetoneacrylamide-co-2-ethylhexyl acrylate-co-methyl methacrylate-co-tetraethyleneglycol dimethacrylate)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
A monomer solution was prepared by uniformly dissolving 158 g of 2-ethylhexyl acrylate, 35.1 g of 2-acetoacetoxyethyl methacrylate, 76.2 g of methyl methacrylate, 80.3 g of diacetoneacrylamide and 1.0 g of tetraethyleneglycol dimethacrylate. After charging 100 g of the monomer solution into a 2-liter four-necked flask provided with a Dimroth condenser, thermometer, nitrogen gas inlet tube and stirrer, 350 g of ethyl acetate was added as a solvent. The temperature was increased to 75 C. while blowing in nitrogen gas at a flow rate of 100 ml/min, and after maintaining a temperature of 75 C. for 30 minutes, 0.35 g of benzoyl peroxide was dissolved in 5 g of ethyl acetate and added as an initiator, and the external temperature was set to 85 C. After confirming reflux of the solvent, the remaining monomer was continuously charged in over a 3 hour period. From one hour after starting continuous charging of the monomer solution, 500 g of ethyl acetate was continuously charged in over a 3 hour period. After charging in ethyl acetate and then continuing to stir for 12 hours, 0.5 g of benzoyl peroxide was charged in as additional catalyst and the mixture was heat treated for 12 hours and then cooled to produce a solution of a non-aqueous acrylic-based pressure-sensitive adhesive.
Synthesis of [2-(3-oxo-1,1-dimethylbutylcarbamoyl)ethyl]bis(pentafluorophenyl)phosphine oxide (Va)
A solution of 1.146 g (3.3 mmol) of acid I in 7 mL of anhydrous ether was added dropwise to a solution of 0.558 g (3.3 mmol) of N-(3-oxo-1,1-dimethylbutyl)acrylamide IVa in 5 mL of anhydrous ether, the mixture was kept for 2 h at ambient temperature and evaporated to dryness. The resultant foam-like residue was triturated with 10 mL of hexane, and the precipitate formed was separated by filtration, washed sequentially with 6 mL of a hexane-ether (1 : 1) mixture and 6 mL of hexane, and dried in air to give 1.514 g of [2-(3-oxo-1,1-dimethylbutylcarbamoyl)ethyl]bis(pentafluorophenyl)phosphine oxide (Va). Yield 91.6%.
Stage #1: N-(2-methyl-4-oxopentan-2-yl)-3-(morpholin-4-yl)propanamide; acetic anhydride In toluene at 20 - 80℃; for 2h; Inert atmosphere;
Stage #2: With 2,6-di-tert-butyl-4-methyl-phenol; triethylamine Reflux;
11 Example 11:
Under argon protection, 11.2 g of acetic anhydride and 25.6 g were addedN - (2-methyl-4-oxapentan-2-yl) -3-morpholinopropionamideThe raw material is mixed with 250 ml of toluene, and the temperature is slowly increased from room temperature to 60 to 80 DEG C and stirred for 2 hours. After stirringMix and then add 0.2 g inhibitor BHT and 0.1 g cuprous chloride and 10.8 g triethylamine, and gradually warmed to reflux reactionNight, the reaction system was concentrated under reduced pressure to give the crude product which was directly separated by silica gel column chromatography with hexane-ethyl acetate14.1 grams of purified pure acrylamide (85% yield) and 9.8 grams of pure N-acetylmorpholine (76% yield).
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