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CAS No. : | 1417713-93-9 | MDL No. : | |
Formula : | C33H30O9 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | OXBIDZVLELTOEU-UHFFFAOYSA-N |
M.W : | 570.59 | Pubchem ID : | 91810419 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P301+P312-P302+P352-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
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 |
---|---|---|
53% | at 85℃; for 72h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 95℃; for 72h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: 1,3,5-tris(bromomethyl)-2,4,6-trimethylbenzene; methyl 3-hydroxybenzoate With potassium carbonate In N,N-dimethyl-formamide at 90℃; for 96h; Stage #2: With water; potassium hydroxide In tetrahydrofuran; ethanol at 90℃; for 6h; | Synthesis of ligand TTBA 5 mmol of compound 1, 15 mmol of compound 2 and45 mmol of K2CO3 were dissolved in 250 ml DMF and then heated to 90 °C andstirred at this temperature for 96 h. After cooling to room temperature, a lot ofwater was added into the above mixture and afforded a large number of precipitates.The precipitate was dissolved in the mixed solvents of 50 ml H2O, 80 mlEtOH and 60 ml THF containing 4.5 g KOH, then the mixture was hydrolyzed at90 °C for 6 h. The solvent was removed and water was added and the pH wastuned to about 3. The white precipitate was obtained and filtered and dried at 60 °C. 1H NMR (DMSO-d6): δ 2.40 (s, 9H), 5.18 (s, 6H), 7.31 (d, 3H), 7.45 (t, 3H),7.56-7.60 (m, 6H), 13.0 (s, 3H) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62% | In formic acid at 140℃; for 72h; Sealed tube; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | Stage #1: 3,3',3”-(((2,4,6-trimethylbenzene-1,3,5-triyl)tris(methylene))tris(oxy))tribenzoic acid; chloro-diphenylphosphine With triethylamine In toluene at 20℃; for 0.166667h; Stage #2: (S)-2-azido-3-phenylpropionic acid methyl ester In toluene at 25℃; for 8h; | 31 Example 31 In the reactor, add 0.2 mmol3,3',3”-(((2,4,6-trimethylbenzene-1,3,5-triyl)tris(methylene))tris(oxy))tribenzoic acid and 1 ml Toluene,Then add 0.6 millimoles of chlorodiphenyl phosphine and 0.72 millimoles of triethylamine, and stir at room temperature for 10 minutes,Add 0.6 millimoles of azide derived from L-phenylalanine methyl ester and react at 25°C for 8 hours,The reaction solution directly used the eluent (V petroleum ether:V ethyl acetate=1:4) to obtain N-acyl phosphoramide compound 6aai through silica gel column chromatography, with a yield of 63%, a colorless oily liquid. |