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[ CAS No. 6061-04-7 ] {[proInfo.proName]}

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Chemical Structure| 6061-04-7
Chemical Structure| 6061-04-7
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Product Details of [ 6061-04-7 ]

CAS No. :6061-04-7 MDL No. :MFCD21337848
Formula : C2HCl2NO2 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W :141.94 Pubchem ID :-
Synonyms :

Safety of [ 6061-04-7 ]

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Application In Synthesis of [ 6061-04-7 ]

* 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.

  • Downstream synthetic route of [ 6061-04-7 ]

[ 6061-04-7 ] Synthesis Path-Downstream   1~32

  • 1
  • [ 120739-77-7 ]
  • [ 6061-04-7 ]
  • 1-[N-(2-chloro-5-pyridylmethyl)-N-n-ethylamino]-1-methylamino-2-nitroethylene [ No CAS ]
YieldReaction ConditionsOperation in experiment
2.9 g (76.5%) With triethylamine; methylamine; In acetonitrile; EXAMPLE 12 A solution of 2.4 g (0.014 mol) of N-(6-chloro-3-pyridyl)methyl-N-ethylamine, 1.4 g (0.014 mol) of triethylamine in 5 ml of acetonitrile was dropwise added to a solution of 2.0 g (0.014 mol) of 1,1-dichloro-2-nitroethylene in 35 ml of acetonitrile at 3-5 C. with stirring. After stirring for 30 minutes, 4.4 g (0.057 mol) of methylamine (40% methanol solution) were added to the reaction mixture and stirred for 30 minutes. The reaction mixture was filtered, and the filtrate was concentrated and purified by a silica gel column chromatography (chloroform/ethanol=7/1) to afford 2.9 g (76.5%) of 1-[N-(6-chloro-3-pyridyl)methyl-N-ethyl]amino-1-methylamino-2-nitroethylene as pale yellowish crystals.
  • 2
  • [ 120739-77-7 ]
  • [ 6061-04-7 ]
  • [ 74-89-5 ]
  • nitenpiram [ No CAS ]
YieldReaction ConditionsOperation in experiment
352.0 g of n-butyl acetate and 102.9 g of a 35% potassium carbonate aqueous solution were charged in a 1-L separable flask. The solution was cooled to 4C, 48.8 g of 1,1-dichloro-2-nitroethene (net weight 40.6 g) was added dropwise while stirring over 30 minutes, and 44.8 g of 2-chloro-5-(ethylaminomethyl)pyridine (net weight 44.4 g) was subsequently added dropwise over 3 hours. The reaction mixture was stirred at -4C for 15 minutes, 60.6 g of a 40% methyl amine solution was added dropwise over 3 hours, and the stirring was further continued for 4 hours. The obtained reaction mixture was warmed to 15C and extracted four times with 51.5 g, 40.3 g, 30.0 g, and 30.0 g of water, and the obtained four extracted aqueous layers were combined. The combined aqueous layer was extracted four times with 75.0 g of 5-ethyl-2-methylpiridine at 15C, and the obtained four extracted 5-ethyl-2-methylpyridine layers were combined (amount of the recovered aqueous layer 1, 247.8 g). After washing the combined 5-ethyl-2-methylpyridine layer with 50.0 g of a saturated sodium sulfate solution (amount of the recovered aqueous layer 2, 66.0 g), 800 g of n-heptane was added thereto and concentrated at 4.5 kPa, 25 to 35C until the amount of the residual solution was 345 g. 20.0 g of 5-ethyl-2-methylpyridine was added to the concentrated mass, and the mixture was maintained at 40C for 1 hour followed by filtration to remove insoluble matters. The obtained filtrate was flushed down with 10.0 g of 5-ethyl-2-methylpyridine to a 500-ml separable flask, the temperature was adjusted to 35C. Then 0.01 g of seed crystals of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N'-methyl-2-nitro-1,1-ethenediamine was added and the mixture was cooled to 15C over 5 hours, and subsequently cooled at -10C over 10 hours for crystallization. The crystalline mass was further stirred at -10C for 3 hours and filtered (recovered filtrate amount, 304.1 g). The obtained crystals were washed with 300.0 g of n-butyl acetate which had been cooled to -10C (recovered washing amount, 305.9 g). The washed crystals were dried at 2.7 kPa, 40C for 4 hours to obtain 45.3 g of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N'-methyl-2-nitro-1,1-ethenediamine at a content of 98.9%
Example 3Synthesis of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N'-methyl-2-nitro-1,1-ethenediamine (third batch)351.9 g of n-butyl acetate and 102.7 g of a 35% potassium carbonate aqueous solution were charged in a 1-L separable flask. The solution was cooled to -4 C., 48.8 g of 1,1-dichloro-2-nitroethene (net weight 40.6 g) was added dropwise while stirring over 30 minutes, and 44.8 g of 2-chloro-5-(ethylaminomethyl)pyridine (net weight 44.4 g) was subsequently added dropwise over 3 hours. The reaction mixture was stirred at -4 C. for 15 minutes, 60.6 g of a 40% methyl amine aqueous solution was added dropwise over 3 hours, and stirring was further continued for 4 hours.The obtained reaction mixture was warmed to 15 C. and extracted four times with the extracted aqueous layers 1, 2 and 3 obtained in Example 2 (50.3 g, 45.2 g, and 31.9 g, respectively) and 30.0 g of water, and the obtained four extracted aqueous layers were combined. The combined aqueous layer obtained was extracted at 15 C. four times with the extracted 5-ethyl-2-methylpyridine layers 1, 2 and 3 obtained in Example 2 (85.5 g, 85.6 g and 90.4 g, respectively) and 75.0 g of 5-ethyl-2-methylpyridine, and the obtained four extracted 5-ethyl-2-methylpyridine layers were combined. After washing the combined 5-ethyl-2-methylpyridine layer with 50.0 g of saturated sodium sulfate solution, 800 g of n-heptane was added thereto and the mixture was concentrated at 4.5 kPa, 25 to 35 C. until the amount of the residual solution was 350.6 g. 20.0 g of 5-ethyl-2-methylpyridine was added to the concentrated mass, and the mixture was maintained at 40 C. for 1 hour followed by filtration to remove insoluble matters.The obtained filtrate was flushed down with 10.0 g of 5-ethyl-2-methylpyridine to a 500 ml separable flask, the temperature was adjusted to 35 C., and then 20.0 g of n-heptane was added dropwise over minutes. 0.01 g of seed crystals of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N'-methyl-2-nitro-1,1-ethenediamine was added to the mass and the mixture was cooled to 15 C. over 5 hours, and subsequently cooled to -10 C. over 10 hours for crystallization. The crystalline mass was further stirred at -10 C. for 3 hours and filtered. The obtained crystals were washed with 60.0 g of 5-ethyl-2-methylpyridine/n-heptane (9/1 weight ratio) which had been cooled to -10 C., and subsequently washed with 200.0 g of n-heptane cooled to -10 C. The washed crystals were dried at 2.7 kPa, 40 C. for 4 hours to obtain 61.4 g of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N'-methyl-2-nitro-1,1-ethenediamine with a content of 99.2%.
  • 3
  • [ 6061-04-7 ]
  • [ 136-64-1 ]
  • C10H9N5O4 [ No CAS ]
  • 4
  • [ 6061-04-7 ]
  • [ 2760-98-7 ]
  • C10H9N5O4 [ No CAS ]
  • 5
  • [ 3645-45-2 ]
  • [ 6061-04-7 ]
  • [ 1445-69-8 ]
YieldReaction ConditionsOperation in experiment
50% In water at 20℃; for 12h; Green chemistry;
  • 6
  • [ 6061-04-7 ]
  • [ 83265-53-6 ]
  • 2-(2-nitroacetamido)-5-(trifluoromethyl)benzoic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
90% In water; at 50℃; for 57h;Green chemistry; General procedure: 2-Aminobenzoic acid (2 mmol) and 1,1-dichloro-2-nitroethene(2.4 mmol) were added to 3 mL of water in a 10 mL round-bottomflask. Then stirred at 50 C, after completion, the product precipitatedfrom the reaction mixture and can be easily separated by filtration,then give the pure product.
  • 7
  • [ 6061-04-7 ]
  • [ 5653-40-7 ]
  • 4,5-dimethoxy-2-(2-nitroacetamido)benzoic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
94% In water at 50℃; for 9h; Green chemistry; General procedure for the preparation of 3a-3h General procedure: 2-Aminobenzoic acid (2 mmol) and 1,1-dichloro-2-nitroethene(2.4 mmol) were added to 3 mL of water in a 10 mL round-bottomflask. Then stirred at 50 C, after completion, the product precipitatedfrom the reaction mixture and can be easily separated by filtration,then give the pure product.
  • 8
  • [ 6061-04-7 ]
  • [ 619-17-0 ]
  • 4-nitro-2-(2-nitroacetamido)benzoic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
91% In water; at 50℃; for 45h;Green chemistry; General procedure: 2-Aminobenzoic acid (2 mmol) and 1,1-dichloro-2-nitroethene(2.4 mmol) were added to 3 mL of water in a 10 mL round-bottomflask. Then stirred at 50 C, after completion, the product precipitatedfrom the reaction mixture and can be easily separated by filtration,then give the pure product.
  • 9
  • [ 6061-04-7 ]
  • [ 4389-45-1 ]
  • 3-methyl-2-(2-nitroacetamido)benzoic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
92% In water at 50℃; for 5h; Green chemistry; General procedure for the preparation of 3a-3h General procedure: 2-Aminobenzoic acid (2 mmol) and 1,1-dichloro-2-nitroethene(2.4 mmol) were added to 3 mL of water in a 10 mL round-bottomflask. Then stirred at 50 C, after completion, the product precipitatedfrom the reaction mixture and can be easily separated by filtration,then give the pure product.
  • 10
  • [ 6061-04-7 ]
  • [ 394-31-0 ]
  • 5-hydroxy-2-(2-nitroacetamido)benzoic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
90% In water; at 50℃; for 12h;Green chemistry; General procedure: 2-Aminobenzoic acid (2 mmol) and 1,1-dichloro-2-nitroethene(2.4 mmol) were added to 3 mL of water in a 10 mL round-bottomflask. Then stirred at 50 C, after completion, the product precipitatedfrom the reaction mixture and can be easily separated by filtration,then give the pure product.
  • 11
  • [ 120739-77-7 ]
  • [ 6061-04-7 ]
  • [ 75-04-7 ]
  • nitenpiram [ No CAS ]
YieldReaction ConditionsOperation in experiment
494.1 kg 1, In the 5000L stainless steel reactor,put disodium hydrogenphosphate 284kg, sodium dihydrogen phosphate, 67.9kg,720kg of tap water was added. Stirred solution becomes clear. At 25 deg.C, then 1500kg of methylene chloride was added, as well as N- (6-chloro - 3-pyridylmethyl) -N- ethylamine 341kg. Cooled 0 deg. C;2, was added dropwise 325 kg of 1,1-dichloro-2-nitroethylene, about 2 ~ 3h, temperature 5 ~ 10 deg.C;3, addition was complete at 5 ~ 10 deg.C. Maintain temperature for 2h; 4, then dropping 40% monomethylamine 390kg,about 2 ~ 3h, and maintain temperature for 2h at 5 ~ 10 deg.C ;5, then heated to 30 deg.C and hold temperature 1h; 6, still 30min, separated and the aqueous layer was further 500kg, extracted once with methylene chloride; 7, the combined organic phases, first at atmospheric pressure and then vacuum recovery methylene chloride, ethyl acetate500kg;8, 0 ~ 5 deg.C cooling crystallization 2h, centrifugal drying drying material, was 494.1kg, HPLC?99.5%,external standard content ?98%, a yield of 0.92.
  • 12
  • [ 6061-04-7 ]
  • [ 1885-32-1 ]
  • 8-methyl-2-(nitromethyl)quinazolin-4(1H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
83% In water; at 70℃; for 3.5h; General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 13
  • [ 6061-04-7 ]
  • [ 437998-34-0 ]
  • 8-bromo-2-(nitromethyl)quinazolin-4(3H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
85% In water; at 70℃; for 2h; General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 14
  • [ 6061-04-7 ]
  • [ 31930-18-4 ]
  • 7-nitro-2-(nitromethyl)quinazolin-4(1H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
85% In water; at 70℃; for 2h; General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 15
  • [ 6061-04-7 ]
  • [ 39549-79-6 ]
  • 7-methyl-2-(nitromethyl)quinazolin-4(1H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
96% In water; at 70℃; for 2h; General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 16
  • [ 6061-04-7 ]
  • [ 5004-88-6 ]
  • 6,7-dimethoxy-2-(nitromethyl)quinazolin-4(1H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
80% In water; at 70℃; for 2h; General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 17
  • [ 6061-04-7 ]
  • [ 5202-85-7 ]
  • 6-chloro-2-(nitromethyl)quinazolin-4(1H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
92% In water at 70℃; for 2h; General Procedure for the Synthesis of 2-(nitromethyl)quinazolin-4(1H)-ones (3a-3l) General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 18
  • [ 6061-04-7 ]
  • [ 54166-95-9 ]
  • 5-chloro-2-(nitromethyl)quinazolin-4(1H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
81% In water at 70℃; for 2h; General Procedure for the Synthesis of 2-(nitromethyl)quinazolin-4(1H)-ones (3a-3l) General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 19
  • [ 6061-04-7 ]
  • [ 115643-59-9 ]
  • 5-fluoro-2-(nitromethyl)quinazolin-4(1H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
87% In water; at 70℃; for 1.5h; General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 20
  • [ 6061-04-7 ]
  • [ 147123-47-5 ]
  • 2-(nitromethyl)thieno[3,2-d]pyrimidin-4(3H)-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
95% In water; at 70℃; for 2h; General procedure: 2-Aminobenzamides (1 mmol) and 1,1-dichloro-2-nitroethene (1.2 mmol) were added to 5 mL of water in a 25 mL round-bottom flask. Then stirred at corresponding temperature and corresponding reaction time, after completion, the product precipitated from the reaction mixture and can be easily separated by filtration, then give the pure products.
  • 21
  • [ 6061-04-7 ]
  • [ 1227-45-8 ]
  • (2Z,4Z)-N,3-bis(4-methoxyphenyl)-4-(nitromethylene)-1,3-thiazetidin-2-imine [ No CAS ]
YieldReaction ConditionsOperation in experiment
73% In ethanol at -25℃;
  • 22
  • [ 6061-04-7 ]
  • [ 1227-45-8 ]
  • (3Z,5Z)-N,2-bis(4-methoxyphenyl)-5-(nitromethylene)-1,4,2-dithiazolidin-3-imine [ No CAS ]
YieldReaction ConditionsOperation in experiment
56% With tetrabutyl ammonium fluoride In chloroform at -10℃;
  • 23
  • [ 6061-04-7 ]
  • [ 1220-00-4 ]
  • (2Z,4Z)-N,3-bis(4-chlorophenyl)-4-(nitromethylene)-1,3-thiazetidin-2-imine [ No CAS ]
YieldReaction ConditionsOperation in experiment
81% In ethanol at -25℃;
  • 24
  • [ 6061-04-7 ]
  • [ 1220-00-4 ]
  • (3Z,5Z)-N,2-bis(4-chlorophenyl)-5-(nitromethylene)-1,4,2-dithiazolidin-3-imine [ No CAS ]
YieldReaction ConditionsOperation in experiment
43% With tetrabutyl ammonium fluoride In chloroform at -10℃;
  • 25
  • [ 6061-04-7 ]
  • [ 2293-07-4 ]
  • (Z)-N-(4-methoxyphenyl)-5-(nitromethylene)-1,4,2-dithiazol-3-amine [ No CAS ]
  • 26
  • [ 6061-04-7 ]
  • [ 1516-37-6 ]
  • (Z)-N-(2-methoxyphenyl)-5-(nitromethylene)-1,4,2-dithiazol-3-amine [ No CAS ]
YieldReaction ConditionsOperation in experiment
45% With tetrabutyl ammonium fluoride In chloroform at -10℃;
  • 27
  • [ 6061-04-7 ]
  • [ 2646-30-2 ]
  • (Z)-N-(4-bromophenyl)-5-(nitromethylene)-1,4,2-dithiazol-3-amine [ No CAS ]
YieldReaction ConditionsOperation in experiment
41% With tetrabutyl ammonium fluoride In chloroform at -10℃;
  • 28
  • [ 6061-04-7 ]
  • [ 614-23-3 ]
  • (Z)-N-(5-(nitromethylene)-1,4,2-dithiazol-3-yl)benzamide [ No CAS ]
YieldReaction ConditionsOperation in experiment
37% With tetrabutyl ammonium fluoride In chloroform at -10℃;
  • 29
  • [ 6061-04-7 ]
  • [ 120740-07-0 ]
  • [ 74-89-5 ]
  • [ 2170133-50-1 ]
YieldReaction ConditionsOperation in experiment
88.6% Stage #1: 1,1-dichloro-2-nitro ethylene; N-((2-chlorothiazol-5-yl)methyl)ethylamine With potassium carbonate In dichloromethane at 0 - 10℃; for 2h; Stage #2: methylamine In water at 5 - 10℃; for 1h; 2 2 In a 500 mL four-necked flask, 35.1 g (89%) of 1,1-dichloronitroethylene (0.22 mol) and 150 mL of dichloromethane were added.Stirring was carried out to 0 to 10 ° C, and 36.2 g (98%) of 2-chloro-5-ethylaminomethylthiazole (0.2 mol) was added dropwise. After the addition, 52 g (40%) of potassium carbonate aqueous solution was added dropwise at this temperature. , keep warm for 2 hours,Sampling HPLC analysis of N-(2-chloro-5-thiazole) methyl-N-ethylamine conversion rate of 98% or more, adding 38.8g (40%) methylamine aqueous solution (0.5mol) at 5-10 °C, plus Stir for 1 hour after finishing.The temperature was raised to 20 to 25 ° C for 2 hours, and the oil layer was separated and allowed to stand, and the aqueous layer was extracted with dichloromethane for 3 times.The oil layer was desolvated, and 70 g of ethyl acetate was added to the residue, stirred well, and cooled to 0 to 5 ° C for filtration.Drying to obtain 50 g of (E)-N-(2-chloro-5-thiazolylmethyl)-N-ethyl-N'-methyl-2-nitrovinylidene diamine, content 98%, yield 88.6% .
  • 30
  • [ 6061-04-7 ]
  • [ 120740-07-0 ]
  • [ 2170133-56-7 ]
YieldReaction ConditionsOperation in experiment
90.1% With potassium carbonate In dichloromethane; water at 0 - 10℃; for 2h; 7 Example 7 31.9 g (89%) of 1,1-dichloronitroethylene (0.2 mol) and 150 mL of dichloromethane were placed in a 500 mL four-necked flask.Stirring was carried out to 0 to 10 ° C, and 75.6 g (98%) of 2-chloro-5-ethylaminomethylthiazole (0.42 mol) was added dropwise. After the addition, 76 g (40%) of potassium carbonate aqueous solution was added dropwise at this temperature. , keep warm for 2 hours,The temperature was raised to 20 to 25 ° C for 2 hours, and the oil layer was separated and allowed to stand, and the aqueous layer was extracted with dichloromethane for 3 times.The combined oil layers were desolvated, and 70 g of ethyl acetate was added to the residue, stirred well, cooled to 0 to 5 ° C, filtered, and dried to obtain 69 g.1,1-bis[N-(2-chloro-5-thiazolylmethyl)-N-ethyl]-2-nitrovinylidene diamine, content 98%, yield 80.1%.
  • 31
  • [ 120739-77-7 ]
  • [ 6061-04-7 ]
  • N-((2-chlorothiazol-5-yl)methyl)ethylamine [ No CAS ]
  • (E)-N-(2-chloro-5-thiazolylmethyl)-N-ethyl-N'-(6-chloro-3-pyridylmethyl)-N'-ethyl-2-nitrovinylidenediamine [ No CAS ]
YieldReaction ConditionsOperation in experiment
83.1% General procedure: This embodiment is basically the same as Embodiment 1, except that:Step 2, using 170 g (15%) sodium carbonate instead of 52 g (40%) potassium carbonate aqueous solution, 41.8 g (98%) <strong>[120739-77-7]2-chloro-5-ethylaminomethylpyridine</strong> instead of 40% methylamine.As a result, 70.5 g of (E)-N-(2-chloro-5-thiazolylmethyl)-N-ethyl-N'-(6-chloro-3-pyridylmethyl)-N'-ethyl-2- Nitrovinylidene diamine, content 98.1%, yield 83.1%. _: 2 In a 500 mL four-necked flask, 35.1 g (89%) of 1,1-dichloronitroethylene (0.22 mol) and 150 mL of dichloromethane were added.Stirring was carried out to 0 to 10 C, and 36.2 g (98%) of 2-chloro-5-ethylaminomethylthiazole (0.2 mol) was added dropwise. After the addition, 52 g (40%) of potassium carbonate aqueous solution was added dropwise at this temperature. , keep warm for 2 hours,Sampling HPLC analysis of N-(2-chloro-5-thiazole) methyl-N-ethylamine conversion rate of 98% or more, adding 38.8g (40%) methylamine aqueous solution (0.5mol) at 5-10 C, plus Stir for 1 hour after finishing.The temperature was raised to 20 to 25 C for 2 hours, and the oil layer was separated and allowed to stand, and the aqueous layer was extracted with dichloromethane for 3 times.The oil layer was desolvated, and 70 g of ethyl acetate was added to the residue, stirred well, and cooled to 0 to 5 C for filtration.Drying to obtain 50 g of (E)-N-(2-chloro-5-thiazolylmethyl)-N-ethyl-N'-methyl-2-nitrovinylidene diamine, content 98%, yield 88.6% .
  • 32
  • [ 120739-77-7 ]
  • [ 6061-04-7 ]
  • C10H11Cl2N3O2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
With ion exchange resin 201×7; In dichloromethane; at -10 - 0℃; for 6h; 1200 kg of dichloromethane was introduced into a 2000 L reactor, and 171 kg (1 kmol) of <strong>[120739-77-7]N-ethyl-2-chloro-5-pyridinemethylamine</strong> was added thereto with stirring, 60 L of ion exchange resin 201×7, and the mixture was cooled to an internal temperature of -10 C, and added dropwise. A solution of 157 kg (1.1 kmol) of 1-dichloro-2-nitroethylene and 320 kg of dichloromethane was added dropwise over 3 hours to control the internal temperature below 0 C. After the dropwise addition, the reaction was kept at 0 C for 3 hours. After the reaction is completed, a solution containing the compound (II) is obtained. The solution was further cooled to an internal temperature of -10 C, and slowly introduced into a methylamine gas of 46.5 kg, (1.5 kmol), controlled internal temperature of 0 C or less, and a calculated amount of monomethylamine gas was passed for 3 hours, and the temperature was maintained at 0 C. 3 hours. After completion, filtration, washing the ion exchange resin with dichloromethane, the filtrate is concentrated to dryness, adding 280 kg of ethyl acetate, stirring and crystallization at room temperature for 1 hour, then cooling to 0 C, stirring and crystallization for 3 hours, centrifuging the feed, drying to obtain the acetamid The amine was 252.3 kg, the purity was 99% or more, and the yield was 93%
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