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CAS No. : | 918633-87-1 | MDL No. : | MFCD22420822 |
Formula : | C9H16Br2N5O4P | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | UGJWRPJDTDGERK-UHFFFAOYSA-N |
M.W : | 449.04 | Pubchem ID : | 11984561 |
Synonyms : |
TH302
|
Chemical Name : | 2-Bromo-N-[(2-bromoethylamino)-[(3-methyl-2-nitroimidazol-4-yl)methoxy]phosphoryl]ethanamine |
Signal Word: | Danger | Class: | 6.1 |
Precautionary Statements: | P201-P261-P280-P305+P351+P338-P308+P313 | UN#: | 2811 |
Hazard Statements: | H315-H317-H319-H335-H360 | Packing Group: | Ⅲ |
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 di-isopropyl azodicarboxylate; triphenylphosphine; In tetrahydrofuran; at 0 - 25℃; for 2h; | [0103j Imidazole alcohol (IA) (1:1.0 w/w), Bromo-IPM (1:2.26 w/w) and triphenylphosphine (1:2.0 w/w) were added to THF (1:13.5 w/v) at 25±5C. The reaction mass was cooled to 0±5C and DIAD (1.5 w/v) was added. The reaction mixture warmed to 25±5C and stirred for 2 hours. Progress of the reaction was monitored by HPLC. Solvent was removed below 50C under vacuum. Solvent exchange with acetonitrile (1:10.0 w/v) below 50C was performed. The syrupy liquid was re-dissolved in acetonitrile (1:10.0 w/v)and the mixture was stirred at -20±5C for 1 hour. The resulting solid was filtered and the filtrate bed was washed with chilled acetonitrile (1:1.0 w/v). The acetonitrile filtrate was concentrated below 50C under vacuum. The concentrated mass was re-dissolved in ethyl acetate (1:10.0 w/v) and concentrated below 50C under vacuum. The ethyl acetate strip off was repeated two more times. Ethyl acetate (1:10.0 w/v) and silica gel (230-400 mesh, 1:5.3w/w) were added to the concentrated reaction mass. The mixture was concentrated below40C under vacuum. n-Heptane (1:5.0 w/v) was charged to the above mass and the mixture was evaporated below 40C under vacuum. n-Heptane (1:5.0 w/v) was again added to the above mass and the solid was filtered and the bed was washed with n-heptane (1:1.0 w/v). The solid was suspended in a mixture of toluene (1:7.1 w/v) and n-heptane (1:21.3 w/v),stirred at 35±5C for 15-20 minutes, filtered off and the bed was washed with n-heptane (1:1.0 w/v). The solid was re-suspended in a mixture of toluene (1:10.6 w/v) and n-heptane (1:10.6 w/v), stirred at 35±5C for 15-20 minutes, filtered off and the bed was washed with nheptane (1:1.0 w/v). The solid was suspended in acetone (1:19.0 w/v), stirred at 35±5C for 15-20 minutes, filtered off and the bed was washed with acetone (1:1.0 w/v). The acetonewashes were repeated 3 more times. Filtrates from the above acetone washings were combined and concentrated below 40C under vacuum. The residue dissolved in ethyl acetate (1:10.0 w/v) and concentrated below 40C under vacuum. The ethyl acetate strip off was repeated one more time. The residue was re-dissolved in ethyl acetate (1:5.5 w/v), cooled to 0±3C and stirred at 0±3C for 2 h and then at -20±5C for 2 h. The solid wasfiltered and the solid was washed with ethyl acetate (1:0.10 w/v). The solid was dissolved in ethyl acetate (1:10.0 w/v) at 50±5C and the resulting solution was filtered through a cartridge filter. The filtrate was concentrated to 4.0 w/w and stirred at 0±3C for 4 hours. The solid was filtered and washed with ethyl acetate (1:0.10 w/v). The crystallization from ethyl acetate was repeated and TH-302 was dried at 25±5C. Table 2 shows how theprocess reduces solvent use. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: sodium hydroxide; water / 17 - 25 °C 2.1: triethylamine / tetrahydrofuran / -15 - 25 °C / Inert atmosphere 2.2: -15 °C 2.3: 0 - 25 °C 3.1: triphenylphosphine; di-isopropyl azodicarboxylate / tetrahydrofuran / 2 h / 0 - 25 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
35% | Phosphorus oxychloride (30.5g, 0.2mol, 1.25eq) was dissolved in 2L of dichloromethane, triethylamine (40.1g, 0.4mol, 2.5eq), 1-methyl-2-nitro-1-imidazole-5-methanol 1d (25g, 0.16mol), after incubating for 1 hour, then add triethylamine (80.2g, 0.8mol, 5.0eq), 2-bromoethylamine hydrobromide ( 122.2g, 0.6mol, 3.75eq).After reacting at room temperature for 2 hours, 1N hydrochloric acid was added to adjust pH = 7, and the liquid was separated. The organic phase was washed with saturated brine (1L × 2), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. To give N, N'-bis (2-bromoethyl) diaminophosphonic acid (1-methyl-2-nitro-1H-imidazol-5-yl) methyl ester (I) (25 g, 56 mmol, white solid ), Yield: 35%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: sodium nitrite; acetic acid / water / 1 h / 0 - 20 °C 2.1: boron; lithium hydride / methanol; tetrahydrofuran / 1 h / 0 °C 3.1: trichlorophosphate; triethylamine / dichloromethane / 1 h 3.2: 2 h / 20 °C |