Category: 1152107-25-9

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 1152107-25-9, name is Gsk-1322322. A new synthetic method of this compound is introduced below., Recommanded Product: Gsk-1322322

Example 8 [(2R)-2-(Cyclopentylmethyl)-3-(2-{5-fluoro-6-[(9aS)-hexahydropyrazino [2,1 -c] [1 ,4] oxazin- 8(1 H)-yl]-2-methyl-4-pyrimidinyl}hydrazino)-3-oxopropyl] hydroxyl formamide dimethanesulphonate. Crystalline [(2R)-2-(Cyclopentylmethyl)-3-(2-{5-fluoro-6-[(9aS)- hexahydropyrazino[2, 1 -c][1 ,4]oxazin-8(1 H)-yl]-2-methyl-4-pyrimidinyl}hydrazino)-3- oxopropyl]hydroxyformamide (100 mg) was dissolved in ethyl acetate (10 ml_). Methanesulphonic acid (40.1 mg) in ethyl acetate (ca. 10 ml.) was prepared. The methanesulphonic acid solution was added dropwise to the solution of freebase in ethyl acetate. A precipitate was formed. The slurry was stirred and aged overnight. The precipitate’s crystallinity was verified by polarized light microscopy. The precipitate and supernatant were separated by filtration. The solids were then vacuum dried. The resulting solid was analytically characterized and found to be Form 1 of the dimethanesulphonate salt of [(2R)-2-(Cyclopentylmethyl)-3-(2-{5-fluoro-6-[(9aS)- hexahydropyrazino[2, 1 -c][1 ,4]oxazin-8(1 H)-yl]-2-methyl-4-pyrimidinyl}hydrazino)-3- oxopropyl]hydroxyformamide by XRPD (see Figure 7). X-Rav Powder Diffraction of r(2R)-2-(Cvclopentylmethyl)-3-(2-f5-fluoro-6-r(9aS)- hexahvdropyrazinor2,1-ciri,41oxazin-8(1 H)-vn-2-methyl-4-pyrimidinyl>hvdrazino)-3- oxopropyUhydroxyformamide dimethanesulphonate The XRPD pattern for polymorphic Form 1 of [(2R)-2-(Cyclopentylmethyl)-3-(2-{5- fluoro-6-[(9aS)-hexahydropyrazino[2, 1 -c][1 ,4]oxazin-8(1 H)-yl]-2-methyl-4- pyrimidinyl}hydrazino)-3-oxopropyl]hydroxyformamide dimethanesulphonate is presented in Figure 7. The X-ray powder diffractogram was collected with a diffraction system utilizing copper Ka radiation, automated divergent slits, nickel Kappabeta filter, and multiple strip detector. Sample presentation consisted of a thin powder layer mounted on a silicon zero background wafer. Thermal Analysis Based on differential scanning calorimetry (DSC) seen in Figure 8 and thermogravimetric analysis (TGA) seen in Figure 9, polymorphic Form 1 of [(2R)-2- (cyclopentylmethyl)-3-(2-{5-fluoro-6-[(9aS)-hexahydropyrazino[2,1 -c][1 ,4]oxazin-8(1 h)-yl]- 2-methyl-4-pyrimidinyl}hydrazino)-3-oxopropyl]hydroxyformamide dimethanesulphonate decomposes at ca. 180 to 185 C under nitrogen.

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Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO. 2) LIMITED; AUBART, Kelly, Marshall; GILLIAN, Jason, Michael; QIN, Donghui; MCKEOWN, Robert, Rahn; WILLIAMS, Glenn, R.; WO2013/82388; (2013); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Related Products of 1152107-25-9, Adding some certain compound to certain chemical reactions, such as: 1152107-25-9, name is Gsk-1322322,molecular formula is C22H34FN7O4, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 1152107-25-9.

Example 10 Synthesis of N-(( ?)-2-(cyclopentylmethyl)-3-(2-(5-fluoro-6-((S)- hexahydro pyrazino[2,1 -c][1,4]oxazin-8(1 H)-yl)-2-methylpyrimidin-4- yl)hydrazinyl)-3-oxopropyl)-N-hydroxyformamide methanesulfonateN-(( ?)-2-(cyclopentylmethyl)-3-(2-(5-fluoro-6-((S)-hexahydropyrazino[2,1- c][1,4]oxazin-8(1 H)-yl)-2-methylpyrimidin-4-yl)hydrazinyl)-3-oxopropyl)-N- hydroxyformamide methanesulfonateTo a 1-L Labmax was added N-(( )-2-(cyclopentylmethyl)-3-(2-(5-fluoro-6-((S)- hexahydropyrazino[2, 1-c][1 ,4]oxazin-8(1 H)-yl)-2-methylpyrimidin-4-yl)hydrazinyl)-3- oxopropyl)-N-hydroxyformamide (100 g, 209 mmol) and n-Propanol (600 mL). The contents were heated to 60C and methanesulfonic acid (13.54 mL, 209 mmol) was added via pipette. Solution was transferred through filter paper and into a clean 1-L Labmax. A rinse of n-propanol (100 mL) was transferred through the filter and into the clean 1-L Labmax. The resulting solution was adjusted to 50C. The solution was seeded with N-((f?)-2-(cyclopentylmethyl)-3-(2-(5-fluoro-6-((S)-hexahydropyrazino[2, 1- c][1 ,4]oxazin-8(1 H)-yl)-2-methylpyrimidin-4-yl)hydrazinyl)-3-oxopropyl)-N- hydroxyformamide methanesulfonate Form 1 (1.0 g, 1.7 mmol). The resulting slurry was aged for 1 hour at 50C. The slurry was cooled to 20C at a linear rate of0.1 C/min. The slurry was aged for 2 hours at 20C. The slurry was cooled to 0C at a linear rate of 0.1 C/min and aged overnight. The slurry was filtered under nitrogen and the cake was washed with chilled n-propanol (100 mL). The resulting wet cake was blown with nitrogen. The wet cake was then dried under vacuum at 50C. After drying, 104 g (86.7% yield) of N-(( )-2-(cyclopentylmethyl)-3-(2-(5-fluoro-6-((S)- hexahydropyrazino[2, 1-c][1 ,4]oxazin-8(1 H)-yl)-2-methylpyrimidin-4-yl)hydrazinyl)-3- oxopropyl)-N-hydroxyformamide methanesulfonate was obtained. H NMR (500 MHz, DMSO-d6, referenced to TMS = 0.00 ppm, T = 25 C, rotamers present due to hindered rotation, major rotamers listed with integration rounded to nearest 1/2 units) delta ppm 10.5-9.7 (3H, several broad s), 9.05 (1/2 H, s), 9.02 (1/2 H, s), 8.31 (1/2 H, s), 7.87 (1/2 H, s), 4.38 (1 H, d, J = 13 Hz), 4.30 (1 H, d, J = 14 Hz), 4.08-4.00 (2H, several m), 3.80-3.72 (3/2 H, several m), 3.56-3.24 (17/2 H, several m), 3.02-2.98 (1 H, m), 2.82-2.69 (1 H, several m), 2.38 (3H, s), 2.26-2.23 (3H, several s), 1.99-1.90 (2H, several m), 1.71 (1 H, broad m), 1.66-1.47, (5H, several m), 1.27- 1.20 (1 H, m), 1.08-1.02 (2H, several m).3C NMR (126 MHz, DMSO-d6, referenced to DMSO-d6 = 39.51 ppm, T = 25 C, rotamers present due to hindered rotation, major rotamers listed with integration rounded to nearest 1/2 units) delta ppm 172.8 (rotamer 1/2 C), 172.7 (rotamer 1/2 C), 162.0 (rotamer 1/2 C), 160.1 (d, J13C-I9F = 9 Hz) (rotamer 1/2 C), 160.0 (d, J13C-I9F = 9 Hz) (rotamer 1/2 C), 157.4 (rotamer 1/2 C), 152.5 (d, J13C-I9F = 10 Hz), 148.2 (broad), 130.4 (d, J13C-19F = 249 Hz) (rotamer 1/2 C), 130.3 (d, J13C-I9F = 249 Hz) (rotamer 1/2 C), 65.2, 63.7, 60.1 , 52.0 (rotamer 1/2 C), 51.7, 51.4, 48.9 (rotamer 1/2 C), 43.8 (broad), 43.4 (broad), 41.2 (rotamer 1/2 C), 41.1 (rotamer 1/2 C), 39.8, 37.0 (rotamer 1/2 C), 36.9 (rotamer 1/2 C), 35.6 (rotamer 1/2 C), 35.5 (rotamer 1/2 C), 32.9, 31.6, 24.9, 24.7 (2C).HRMS (ESI): calcd for C22H35FN704[M + H]+ 480.2730, found 480.2731.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 1152107-25-9, Gsk-1322322, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY NO 2 LIMITED; BULLOCK, Kae Miyake; DESCHAMPS, Nicole; ELITZIN, Vassil; FITZGERALD, Russell; GRADDY, William Hawthorne; MATSUOKA, Richard Tadao; MCKEOWN, Robert Rahn; MITCHELL, Mark Bryan; SHARP, Matthew Jude; SUTTON, Peter W.; TABET, Elie Amine; ZHOU, Xiaoming; WO2014/141181; (2014); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia