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[ CAS No. 1231930-82-7 ] {[proInfo.proName]}

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Cat. No.: {[proInfo.prAm]}
Chemical Structure| 1231930-82-7
Chemical Structure| 1231930-82-7
Structure of 1231930-82-7 * Storage: {[proInfo.prStorage]}
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Product Details of [ 1231930-82-7 ]

CAS No. :1231930-82-7 MDL No. :MFCD25562906
Formula : C28H36F2N8O3S Boiling Point : -
Linear Structure Formula :- InChI Key :NCJPFQPEVDHJAZ-UHFFFAOYSA-N
M.W : 602.70 Pubchem ID :71576678
Synonyms :

Safety of [ 1231930-82-7 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P305+P351+P338 UN#:N/A
Hazard Statements:H302-H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 1231930-82-7 ]

* 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 [ 1231930-82-7 ]

[ 1231930-82-7 ] Synthesis Path-Downstream   1~9

  • 1
  • [ 75-75-2 ]
  • [ 1231929-97-7 ]
  • [5-(4-ethylpiperazin-1-ylmethyl)pyridin-2-yl]-[5-fluoro-4-(7-fluoro-3-isopropyl-2-methyl-3H-benzoimidazol-5-yl)pyrimidin-2-yl]amine methanesulfonate [ No CAS ]
YieldReaction ConditionsOperation in experiment
In methanol; dichloromethane; for 1h; Example 16[5-(4-Ethyl-piperazin-1-ylmethyl)-pyridin-2-yl]-[5-fluoro-4-(7-fluoro-3-isopropyl-2-methyl-3H-benzoimidazol-5-yl)-pyrimidin-2-yl]-amine methanesulfonateAdd methanosulfonic acid (63.59 mL) to a solution of <strong>[1231929-97-7][5-(4-ethyl-piperazin-1-ylmethyl)-pyridin-2-yl]-[5-fluoro-4-(7-fluoro-3-isopropyl-2-methyl-3H-benzoimidazol-5-yl)-pyrimidin-2-yl]-amine</strong> (17.3 g) in a mixture of DCM (100 mL) and methanol (100 mL). Stir the solution for 1 h and remove the solvent under vacuum. Triturate with MtBE and filtrate the solid to afford 20.4 g of the title compound. MS (ES+): m/z=507 (M+H)+.
20.4 g In methanol; dichloromethane; for 1h; Add methanosulfonic acid (63.59 mL) to a solution of [5-(4-ethyl-piperazin-l- ylmethyl)-pyridin-2-yl]-[5-fluoro-4-(7-fluoro-3-isopropyl-2-methyl-3H-benzoimidazol-5- yl)pyrimidin-2-yl] -amine (17.3 g) in a mixture of dichloromethane (100 mL) and methanol (100 mL). Stir the solution for 1 hour and remove the solvent under vacuum. Triturate with methyl tert-butyl ether and filtrate the solid to afford 20.4 g of the title compound. MS 35(ES+): m/z=507 (M+H)+.
  • 2
  • [ 75-75-2 ]
  • [ 1180132-17-5 ]
  • [ 1231930-42-9 ]
  • [5-(4-ethylpiperazin-1-ylmethyl)pyridin-2-yl][5-fluoro-4-(7-fluoro-3-isopropyl-2-methyl-3H-benzoimidazol-5-yl)pyrimidin-2-yl]-amine methanesulfonate [ No CAS ]
YieldReaction ConditionsOperation in experiment
56.65 g Compound 9 (24.23 g, 110 mmol) and toluene (160 mL) were added to a three-neck flask. Stir well and cool to -5 to 0 C. Add hexamethylsilylamine lithium tetrahydrofuran solution (1.0 M, 120 mL, 120 mmol), After stirring at low temperature for 30 to 45 minutes, compound 5 (32.27 g, 100 mmol) was added dropwise. After the addition is completed, the temperature is raised to room temperature at 25 to 30 C for 10 to 16 hours. At the end of the reaction, saturated ammonium chloride (323 mL) was added. Extracted 3 times with ethyl acetate (160 mL). The organic phase was washed twice with saturated brine (160 mL). Dry over anhydrous sodium sulfate, After concentration, it was recrystallized from methylene chloride ethyl acetate mixture to afford compound 10 (43.57 g, 86%).Compound 10 (50.66 g, 100 mmol) was added to a three-necked flask. Add absolute ethanol (251 mL), After stirring and stirring, methanesulfonic acid (14.42 g, 150 mmol) was added. After the addition is completed, the temperature is raised to 50 to 55 C for 4 to 5 hours. The reaction was slowly cooled to 0 to 5 C for 1 hour. filter, The solid was washed with ethanol (50 mL). dry, The product Abemaciclib methanesulfonate 11 (56.65 g, 94%) was obtained.
  • 3
  • [ 53939-30-3 ]
  • [ 1231930-82-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 4 steps 1.1: isopropylmagnesium chloride / tetrahydrofuran / -10 - 0 °C / Inert atmosphere 1.2: 20 °C / Inert atmosphere 2.1: trimethyl orthoformate; formic acid / acetonitrile / Reflux 3.1: copper(l) iodide; potassium carbonate; ammonium hydroxide / 1,2-dimethoxyethane / 110 - 115 °C / Sealed tube 4.1: lithium hexamethyldisilazane / toluene; tetrahydrofuran / -5 - 0 °C 4.2: 25 - 30 °C 4.3: 50 - 55 °C
  • 4
  • [ 23100-12-1 ]
  • [ 1231930-82-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 3 steps 1.1: trimethyl orthoformate; formic acid / acetonitrile / Reflux 2.1: copper(l) iodide; potassium carbonate; ammonium hydroxide / 1,2-dimethoxyethane / 110 - 115 °C / Sealed tube 3.1: lithium hexamethyldisilazane / toluene; tetrahydrofuran / -5 - 0 °C 3.2: 25 - 30 °C 3.3: 50 - 55 °C
  • 5
  • [ 5308-25-8 ]
  • [ 1231930-82-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 3 steps 1.1: trimethyl orthoformate; formic acid / acetonitrile / Reflux 2.1: copper(l) iodide; potassium carbonate; ammonium hydroxide / 1,2-dimethoxyethane / 110 - 115 °C / Sealed tube 3.1: lithium hexamethyldisilazane / toluene; tetrahydrofuran / -5 - 0 °C 3.2: 25 - 30 °C 3.3: 50 - 55 °C
  • 6
  • [ 658072-14-1 ]
  • [ 1231930-82-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 4 steps 1.1: triethylamine / acetonitrile / 90 - 95 °C / Sealed tube 2.1: toluene-4-sulfonic acid / toluene / Reflux 3.1: isopropylmagnesium chloride / tetrahydrofuran / 0 - 5 °C / Inert atmosphere 3.2: 55 - 60 °C / Inert atmosphere 4.1: lithium hexamethyldisilazane / toluene; tetrahydrofuran / -5 - 0 °C 4.2: 25 - 30 °C 4.3: 50 - 55 °C
  • 7
  • [ 2377540-91-3 ]
  • [ 1231930-82-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 3 steps 1.1: toluene-4-sulfonic acid / toluene / Reflux 2.1: isopropylmagnesium chloride / tetrahydrofuran / 0 - 5 °C / Inert atmosphere 2.2: 55 - 60 °C / Inert atmosphere 3.1: lithium hexamethyldisilazane / toluene; tetrahydrofuran / -5 - 0 °C 3.2: 25 - 30 °C 3.3: 50 - 55 °C
  • 8
  • [ 1231930-33-8 ]
  • [5-(4-ethylpiperazin-1-ylmethyl)pyridin-2-yl][5-fluoro-4-(7-fluoro-3-isopropyl-2-methyl-3H-benzoimidazol-5-yl)pyrimidin-2-yl]-amine methanesulfonate [ No CAS ]
  • 9
  • [ 75-75-2 ]
  • [ 1231929-97-7 ]
  • [ 1231930-82-7 ]
YieldReaction ConditionsOperation in experiment
In dichloromethane at 20℃; 1-9 Example 1 (0165) 500 mg abemaciclib was dissolved in 2 mL dichloromethane to form a clear solution, the solution was stirred at room temperature and 1 mL dichloromethane solution containing 96.2 mg methanesulfonic acid was dripped in, then 5 mL isopropyl ether was added, white solid appeared; 3 days after stirring, the obtained solid was filtrated and vacuum dried at 40° C., and abemaciclib mesylate Form 1 was obtained. (0166) Its XRPD pattern is shown in FIG. 1. (0167) Its DSC thermogram is shown in FIG. 2. (0168) Its TGA thermogram is shown in FIG. 3. (0169) The 1H-NMR (DMSO) data of the product are as follows: (0170) 1H-NMR (500 MHz, DMSO-d6): δ10.18 (s, 1H), 8.71 (d, J=3.7 Hz, 1H), 8.28 (s, 1H), 8.27-8.20 (m, 2H), 7.71 (t, J=10.3 Hz, 2H), 4.85 (hept, J=6.9 Hz, 1H), 3.59 (s, 2H), 3.13 (s, 2H), 3.04-2.89 (m, 4H), 2.65 (s, 3H), 2.33 (s, 3H), 1.63 (d, J=6.9 Hz, 6H), 1.21 (t, J=7.3 Hz, 3H). It indicates that the compound is abemaciclib mesylate.
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