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CAS No. : | 58909-39-0 | MDL No. : | MFCD00185756 |
Formula : | C4H5N3O2S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | UMWWHOXOVPIGFD-UHFFFAOYSA-N |
M.W : | 159.17 | Pubchem ID : | 3034640 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H319 | 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 |
---|---|---|
With sodium acetate; In methanol; dichloromethane; water; | Ceftriaxone-One Pot Procedure 23.87 g of cefotaxime in free form and 7.95 g of 3-mercapto-2-methyl-(2,5-dihydro-6-hydroxy-5-oxo-as)-triazin in 150 ml of dichloromethane are treated with 57.92 g of BSTFA while stirring under inert gas. A solution obtained is refluxed for several hours, cooled in an ice-bath, and treated with 33.34 g of TMSTf. The mixture obtained is poured onto an ice-cooled solution of 20.5 g of sodium acetate in 350 ml of methanol/water and 250 ml of water and 500 ml of dichloromethane are added. Further treatment and work-up is carried out according to the method describred in example 8. Disodium ceftriaxone is obtained in a purity of 99.6% (HPLC, area). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
[A] 3-Mercapto-2,5-dihydro-2-methyl-5-oxo-6-hydroxy -1,2,4-triazine NMR(D2 O)delta; 3.43(2H,ABq), 3.69(3H,s), 4.22(2H,ABq), 5.16(lH,d), 5.33(2H,ABq), 5.82(lH,d), 6.86(lH,s), 7.11(lH,s), 7.74(lH,s) | ||
(A) 3-Mercapto-2,5-dihydro-2-methyl-5-oxo-6-hydroxy-1,2,4-triazine NMR(D2 O) delta: 3.50(1/2*2H, ABq), 3.58(1/2*2H, ABq), 3.65, 3.66(each 1/2*3H, s), 4.21(1/2*2H, ABq), 4.24(1/2*2H, ABq), 5.04(1H, s), 5.10(1/2H, d), 5.14(1/2H, d), 5.63(1/2H, d), 5.72(1/2H, d), 6.75(1/2H, s), 6.80(1/2H, s), 7.35(1/2H, s), 7.36(1/2H, s), 7.58(1H, s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine; In tetrahydrofuran; | (A) A solution of 2-methyl-3-mercapto-6-hydroxy-2,5-dihydro-1,2,4-triazin-5-one (0.8 g) in dry tetrahydrofuran (25 ml) was stirred for 30 min with triethylamine (0.835 ml) and tert-butyldiphenylsilylchloride (1.53 ml). The reaction mixture was partitioned between 1% aqueous NaHCO3 and ethyl acetate. Removal of the solvent from the dried organic layer left a residue which crystallized by trituration with light petrol affording 2-methyl-3-mercapto-6-tert-butyldiphenylsilyloxy-2,5-dihydro-1,2,4-triazin-5-one (1.34 g), m.p. 135 C. (decomp.). UV (CHCl3) lambdamax: 276 (epsilon=20,820) and 320 sh (=4,460) nm. IR (CHCl3) gammamax 1720, 1580 cm-1. NMR (CDCl3) deltappm: 1.1 (9H, s), 3.4 (3H, s), 7.2-7.7 (10H, m), 9.9 (1H, br s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With TMSI; acetic acid; In tetrahydrofuran; dichloromethane; water; dimethyl sulfoxide; acetonitrile; | EXAMPLE 2 7beta-[2-(2-Aminothiazol-4-yl)-2-(4-chlorobenzyloxyimino)acetamido]-3-[(2,5-dihydro-6-hydroxy-2-methyl-5-oxo-1,2,4-triazin-3-yl)thiomethyl]-3-cephem-4-carboxylic acid To a suspension of 200 mg (0.35 mmole) of 7beta-[2-(2-aminothiazol-4-yl)-2-(4-chlorobenzyloxyimino)acetamido]-3-acetoxymethyl-3-cephem-4-carboxylic acid in 5 ml of methylene chloride was added 0.5 ml of MSTFA and the suspension was stirred at 40 C. until solution occurred. The solution was cooled to room temperature and 0.13 ml (0.87 mmole) of TMSI was added. The reaction stirred at room temperature for 30 minutes and evaporated to an oil. The oil was dissolved in 3 ml of acetonitrile and 0.12 ml (1.5 mmole) of THF was added. The mixture was then stirred at room temperature for 5 minutes to destroy excess TMSI and provide in solution the corresponding 3-iodomethyl-3-cephem derivative. To the solution of the 3-iodomethyl-3-cephem was added a solution of 65 mg (0.4 mmole) of 2,5-dihydro-6-hydroxy-2-methyl-5-oxo-1,2,4-triazine-3-thiol in 1 ml of acetonitrile, prepared with 0.25 ml of MSTFA, and the mixture was stirred at room temperature for 3 hours. The reaction mixture then was treated with three drops of water, the precipitate filtered and dried to yield 240 mg of crude title compound. The product was dissolved in DMSO and chromatographed over a C18 reverse phase column using 30% acetonitrile:water:2% acetic acid for elution. The fractions containing the product were combined, concentrated to a small volume by evaporation, and the concentrate lyophilized to yield 100 mg of the title compound. IR: 1772 cm-1 (beta-lactam carbonyl). UV: lambdamax 225 epsilon29855. MS (FAB): M+ 665. |
[ 117829-36-4 ]
3-Amino-2-thioxoimidazolidin-4-one
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