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CAS No. : | 57-96-5 | MDL No. : | MFCD00057279 |
Formula : | C23H20N2O3S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MBGGBVCUIVRRBF-UHFFFAOYSA-N |
M.W : | 404.48 | Pubchem ID : | 5342 |
Synonyms : |
G-28315;NSC 75925;Anturanil;Anturane;(+/-)-Sulfinpyrazone
|
Chemical Name : | 1,2-Diphenyl-4-(2-(phenylsulfinyl)ethyl)pyrazolidine-3,5-dione |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302 | Packing Group: | N/A |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
0.5 mg anagrelide, 50 mg zomepirac. Sulfinpyrazone: | ||
The method of claim 1 wherein said compound is selected from the group consisting of:...4-butyl-1-(p-hydroxyphenyl)-2-phenyl-3,5-pyrazolidinedione4-(3-hydroxybutyl)-1,2-diphenyl-3,5-pyrazolidinedione4-butyl-1-(p-hydroxyphenyl)-2-phenyl-3,5-pyrazolidinedione4-(3-hydroxy)-1-(p-hydroxyphenyl)-2-phenyl-3,5-pyrazolidinedione4-[2-(phenylsulfinyl)ethyl]-1,2-diphenyl-3,5-pyrazolidinedione4-[2-(phenylthio)ethyl]-1,2-diphenyl-3,5-pyrazolidinedione. | ||
Examples of compounds coming within the scope of the invention include:...4-butyl-1-(p-hydroxyphenyl)-2-phenyl-3,5-pyrazolidinedione (oxyphenbutazone)4-(3-hydroxybutyl)-1,2-diphenyl-3,5-pyrazolidinedione (hydroxyphenylbutazone)4-butyl-1-(p-hydroxyphenyl)-2-phenyl-3,5-pyrazolidinedione (gamma-hydroxyphenylbutazone)4-(3-hydroxy)-1-(p-hydroxyphenyl)-2-phenyl-3,5-pyrazolidinedione (p, gamma-dihydroxyphenylbutazone)4-[2-(phenylsulfinyl)ethyl]-1,2-diphenyl-3,5-pyrazolidinedione (sulfinpyrazone)4-[2-(phenylthio)ethyl]-1,2-diphenyl-3,5-pyrazolidinedione (thio analogue of sulfinpyrazone) STR4 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With sodium hydrogencarbonate; sodium hydrogensulfite; In water; acetic acid; ethyl acetate; toluene; | EXAMPLE 2 Oxidation of 1,2-Diphenyl-4-[2-(phenylthio)ethyl]-3,5-pyrazolidinedione 1,2-Diphenyl-4-[2-(phenylthio)ethyl]-3,5-pyrazolidinedione (20 g, 0.052 moles) was dissolved in 400 ml of glacial acetic acid. To this solution, 240 ml of Caro's acid solution (described in Example 1) was added dropwise over a 30 minute period. A TLC taken three hours after the addition was begun showed starting material. The remainder of the Caro's acid solution was added and the reaction mixture was kept at 5° C. for eighteen hours. Thereafter, the reaction mixture was stirred for two more hours while it came to room temperature. TLC showed no starting material. A 5percent sodium bisulfite solution (200 ml) was added to the reaction mixture followed by the addition of 300 ml of ethyl acetate. Water (500 ml) and 300 ml more of ethyl acetate were added. The layers were separated and the organic layer was washed with 500 ml of 5percent sodium bicarbonate solution. The solvent was evaporated under reduced pressure and toluene (150 ml) was added. The toluene was removed by evaporation under reduced pressure to give a residue (20.2 g). The residue was crystallized from ethanol (60 ml) to give 9.7 g of 1,2-diphenyl-4-[2-(phenylsulfinyl)ethyl]-3,5-pyrazolidinedione. The mother liquors were concentrated to give another 2.8 g of the sulfinyl compound (total 12.5 g, 60percent of theory). The sulfinyl compound exhibited the following characteristics: mp 130°-131.5° C.; nmr(CDCl3)delta 2.45 (m, 2H), 3.3 (m, 3H), 7.25 (m, 10H) and 7.5 (m, 5H); and Anal. Calcd for C23 H20 O 3 N2 S: C, 68.30percent H, 4.99percent N, 6.93percent and Found: C, 67.94percent H, 5.09percent N, 6.84percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In methanol; | (a) 1,2-Diphenyl-4-[2-(phenylsulfinyl)ethyl]-4-hydroxymethyl-pyrazolidine-3,5-dione (II) 40percent Formaline (25 ml) is added to a solution of 20 grams of 1,2-diphenyl-4-[2-(phenylsulfinyl)-ethyl]-pyrazolidine-3,5-dione in 120 ml of methanol. The solution, under magnetic stirring, is heated up to 50° C. for one hour and kept, always under a magnetic stirring, at room temperature for 12 hours. At the end the solvent is evaporated under reduced pressure, the residue is washed with water and extracted with dichloromethane. The organic phase is dried on anhydrous sodium sulphate and the crude product obtained after the solvent evaporation is purified on silica gel chromatographic column, eluent ethyl acetate. The product obtained has m.p. 144°-145° C. Elemental analysis: for C24 H22 N2 SO4 (M.W.=434): calc. percent C=66.36; H=5.07; N=6.45. found percent C=66.22; H=5.21; N=6.38. |