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[ CAS No. 84647-20-1 ] {[proInfo.proName]}

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Chemical Structure| 84647-20-1
Chemical Structure| 84647-20-1
Structure of 84647-20-1 * Storage: {[proInfo.prStorage]}
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Product Details of [ 84647-20-1 ]

CAS No. :84647-20-1 MDL No. :MFCD08062952
Formula : C7H7N3 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 133.15 Pubchem ID :-
Synonyms :

Safety of [ 84647-20-1 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P264-P270-P271-P280-P301+P310-P302+P352-P304+P340-P305+P351+P338-P312-P330-P362-P403+P233-P501 UN#:N/A
Hazard Statements:H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 84647-20-1 ]

* 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 [ 84647-20-1 ]

[ 84647-20-1 ] Synthesis Path-Downstream   1~6

  • 2
  • [ 28900-10-9 ]
  • [ 84647-20-1 ]
YieldReaction ConditionsOperation in experiment
82% With ammonia; In ethanol; at 130℃; for 20h; Example 9; 4-[4-(4-Methoxy-benzyloxy)-2-(7-methyl-pyrido[2,3-d]pyrimidin-4-ylamino)-phenylsulfanyl]-phenol; Example 9A; 2-Amino-6-methyl-nicotinonitrile; [0297] 2-Chloro-6-methyl-nicotinonitrile (25 g, 0.164 mol) and liquid ammonia (250 mL) in 500 mL of ethanol were reacted in a sealed high-pressure vessel at 1300C for 20 hours. The reaction mixture was concentrated under vacuum and the residue washed with water (2 x 50 mL) then dried in a vacuum oven for 24 hours to provide the title compound as a light yellow solid (18 g, 82%). 1H <n="79"/>NMR (300 MHz, DMSO-d6) delta ppm:2.30 (s, 3H), 6.52 (d, J= 7.7 Hz, IH), 6.78 (s, 2H), 7.73 (d, J= 7.7 Hz, IH).
82% With ammonia; In ethanol; at 130℃; for 20h; 2-Chloro-6-methyl-nicotinonitrile (25 g, 0.164 mol) and liquid ammonia (250 mL) in500 mL of ethanol were reacted in a sealed high-pressure vessel at 1300C for 20 hours. The reaction mixture was concentrated under vacuum and the residue washed with water (2 x 50 mL) then dried in a vacuum oven for 24 hours to provide the title compound as a light yellow solid (18 g, 82%). 1H NMR (300 MHz, DMSOd6) delta ppm:2.30 (s, 3H), 6.52 (d, J= 7.7 Hz, IH), 6.78 (s, 2H), 7.73 (d, J= 7.7 Hz, IH).
70% With ammonia; In ethanol; at 180℃; for 60h;Autoclave; 1 ) <strong>[28900-10-9]2-chloro-6-methylnicotinonitrile</strong> (2.00 g, 13.1 mmol) was dispersed in 12 ml of absolute ethanol, saturated with ammonia, and placed in a high-pressure autoclave. The reaction mixture was heated to 180 C for 60 h. Then, after cooling to room temperature, the solvent was evaporated under reduced pressure. The crude product was recrystallized from ethanol obtaining 2-amino-6- methylnicotinonitrile in 70% yield.
70% With ammonia; In ethanol; at 180℃; for 60h;Autoclave; 1) <strong>[28900-10-9]2-chloro-6-methylnicotinonitrile</strong> (2.00 g, 13.1 mmol) was dispersed in 12 ml of absolute ethanol, saturated with ammonia, and placed in a high-pressure autoclave. The reaction mixture was heated to 180 C. for 60 h. Then, after cooling to room temperature, the solvent was evaporated under reduced pressure. The crude product was recrystallized from ethanol obtaining 2-amino-6-methylnicotinonitrile in 70% yield.
41% With ammonia; In ethanol; at 170℃; for 15h; Ammonia was blown into ethanol (50 mL)A solution of saturated ammonia in ethanol (about 10%) was prepared. 2-Chloro-3-cyano-6-methylpyridine (3.05 g) was added thereto and reacted in an autoclave at 170 C for 15 hours. The reaction solution was cooled to room temperature and concentrated under reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate, dried over anhydrous sodium sulfate, and concentrated. The resulting residue was purified by silica gel column chromatography (gradient of hexane: ethyl acetate = 9: 1 to 1: 9) to obtain 2-amino-3-cyano-6-methylpyridine 1.10 g (41%).To the resulting 2-amino-3-cyano-6-methylpyridine 1.10 g was added 15% potassium hydroxide (10 mL)The mixture was stirred at 100 C for 3 hours. The reaction solution was cooled to room temperature, and the pH value was adjusted to 4 to 5 by adding 4 N hydrochloric acid dropwise. The precipitated crystals were collected by filtration, washed further with water and air-dried.obtainAmino-6-methylnicotinic acid 1.18 g (94% yield). The overall yield was 38.5%.

  • 3
  • [ 2976-86-5 ]
  • [ 55244-11-6 ]
  • [ 84647-20-1 ]
  • 5
  • [ 84647-20-1 ]
  • [ 100524-09-2 ]
YieldReaction ConditionsOperation in experiment
94% With potassium hydroxide; at 100.0℃; for 3.0h; Ammonia was blown into ethanol (50 mL)A solution of saturated ammonia in ethanol (about 10%) was prepared. 2-Chloro-3-cyano-6-methylpyridine (3.05 g) was added thereto and reacted in an autoclave at 170 C for 15 hours. The reaction solution was cooled to room temperature and concentrated under reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate, dried over anhydrous sodium sulfate, and concentrated. The resulting residue was purified by silica gel column chromatography (gradient of hexane: ethyl acetate = 9: 1 to 1: 9) to obtain 2-amino-3-cyano-6-methylpyridine 1.10 g (41%).To the resulting 2-amino-3-cyano-6-methylpyridine 1.10 g was added 15% potassium hydroxide (10 mL)The mixture was stirred at 100 C for 3 hours. The reaction solution was cooled to room temperature, and the pH value was adjusted to 4 to 5 by adding 4 N hydrochloric acid dropwise. The precipitated crystals were collected by filtration, washed further with water and air-dried.obtainAmino-6-methylnicotinic acid 1.18 g (94% yield). The overall yield was 38.5%.
  • 6
  • [ 84647-20-1 ]
  • [ 124-38-9 ]
  • [ 36075-35-1 ]
YieldReaction ConditionsOperation in experiment
92% With 1,5-diazabicyclo[4.3.0]non-5-ene 2,2,2-trifluoroethanol; at 60.0℃; for 3.0h; Compound 1b (1 mmol, 133 mg), [HDBN+][TFE-] (6 mmol, 1.35 g) was added to a 10 ml round bottom flask. In a CO2 environment, the reaction is heated to 60C for 3 hours, and the reaction is stopped. After the temperature is cooled to room temperature, a saturated aqueous NH4Cl solution is added. Adjust the pH to neutral, extract three times with 20ml CH2Cl2, collect the CH2Cl2 solution and dry it over anhydrous sodium sulfate. After filtration, the solution was removed by evaporation under reduced pressure, and the resulting solid was separated by silica gel column chromatography (eluent: CH2Cl2:CH3OH=15:1).163 mg of white solid compound 2b, yield 92%.
92% With 1,5-diazabicyclo[4.3.0]non-5-ene 2,2,2-trifluoroethanol; at 60.0℃; under 760.051 Torr; for 3.0h;Green chemistry; General procedure: Substrate (1.0 mmol), [HDBN+][TFE-] (6.0 mmol) were loaded in a 10 mL glass reaction tube equipped with a magnetic stirrer. The air in the reactor was replaced by CO2. Then, the reactor was stirred at the desired temperature for 3-96 h under CO2 using a balloon. After the reaction, the reaction liquid was cooled to room temperature and quenched by saturated ammonium chloride solution. Then the mixture was filtered to afford the crude product, which was purified by chromatography (silica gel, methanol/dichloromethane=1/20) to give the desired compound. The purified product was characterized by NMR and HR-MS. 1H NMR and 13C NMR studies were carried out with a JEOL NMR 400 (400 MHz, 100 MHz) spectrometer with DMSO-d6 as the solvent. Mass spectra were recorded with an AMD40223(Interambulacra) spectrometer.
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