As the paragraph descriping shows that 10049-08-8 is playing an increasingly important role.
In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.10049-08-8, name is Ruthenium(III) chloride An updated downstream synthesis route of 10049-08-8 as follows., 10049-08-8
Example 13 Synthesis of (3S)-3-(1,3-benzodioxol-5-yl)-3-[({1-[2-oxo-3-(phenylmethyl)-1(2H)-pyridinyl]cyclohexyl}carbonyl)amino]propanoic Acid Step One: To a solution of 3-benzylpyridine (1.65 g, 9.77 mmol) in acetone (3.5 mL), 1-chloro-2,4-dinitrobenzene (2.00 g, 9.56 mmol) was added and the mixture was refluxed overnight. The mixture was cooled to room temperature, diluted with acetone and the solvent was decanted from the precipitate. The crude solid was washed with acetone (2 times) and diethyl ether (1 time), decanting each time to give 37(3.57 g, 100percent) as a gray solid. Step Two: To a solution of 1-amino-1-hydroxymethylcyclohexane (0.45 g, 3.5 mmol) in n-butanol (8.75 mL), solid N-(2,4-dintrophenyl)-3-benzylpyridinum chloride (37, 1.23 g, 3.3 mmol) was added. The resulting solution was heated to reflux for 2.5 days under a nitrogen atmosphere. The mixture was cooled, diluted with water and filtered. The filtrate was basified with concentrated NH4OH (2 mL) and extracted with ethyl acetate. The aqueous layer was concentrated to dryness to give 38(0.56 g) as a yellow oil which was used without further purification. Step Three: To a solution of crude 38(0.56 g, 3.5 mmol theoretical) in water (10 mL), a solution of potassium ferricyanide (3.3 g, 10 mmol) in water (15 mL) was added dropwise via an addition funnel over 30 minutes at 0¡ã C. A solution of KOH (0.76 g, 13.5 mmol) in water (5 mL) was then added over 30 minutes. Toluene (10 mL) was added and the solution was stirred for one hour at 0¡ã C. The layers were separated, and the aqueous layer was extracted again with toluene. The combined extracts were dried over Na2SO4 and filtered and the filtrate was concentrated under reduced pressure. The residue was chromatographed on silica gel, eluding with 7:13 hexanes:ethyl acetate to give 39(20 mg, 1.9percent, two steps.) Step Four: To a suspension of 39(20 mg, 0.068 mmol) in aqueous KOH (1M, 0.70 mL) potassium persulfate (0.073 g, 0.270 mmol) and ruthenium (III) chloride (1 mg, catalytic) and THF (0.25 mL) were added. The mixture was stirred for 1 hour and extracted with dichloromethane. The aqueous layer was acidified and extracted with ethyl acetate (3 times). The ethyl acetate extracts were combined, dried over MgSO4 and filtered. The filtrate was concentrated under reduced pressure to give 40(0.0148 g, 70percent) as a tan solid. (3S)-3-(1,3-Benzodioxol-5-yl)-3-[({1-[2-oxo-3-(phenylmethyl)-1(2H)-pyridinyl]cyclohexyl}carbonyl)amino]propanoic acid was prepared from 40according to the procedures described in Example 1. 1H NMR (400 MHz, CD3SO2CD3): delta 1.40 (m, 4H), 1.68 (m, 2H), 2.04 (m, 2H), 2.60 (d, J=7.0 Hz, 2H), 3.67 (d, J=15.2 Hz, 1H), 3.72 (d, J=15.2 Hz, 1H), 5.12 (m, 1H), 5.95 (m, 2H), 6.19 (t, J=7.0 Hz, 1H), 6.74 (dd, J=7.8, 1.4 Hz, 1H), 6.76 (d, J=7.8 Hz, 1H), 6.90 (d, J=1.4 Hz, 1H), 7.10 (d, J=5.8 Hz, 1H), 7.20 (m, 5H), 7.57 (d, J=8.4Hz, 1H), 7.66 (dd, J=7.7, 1.8 Hz, 1H).
As the paragraph descriping shows that 10049-08-8 is playing an increasingly important role.
Reference£º
Patent; Biediger, Ronald J.; Dupre, Brian; Hamaker, Linda K.; Holland, George W.; Kassir, Jamal M.; Li, Wen; Market, Robert V.; Nguyen, Noel; Scott, Ian L.; Wu, Chengde; Decker, E. Radford; US2003/199692; (2003); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI