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CAS No. : | 4845-50-5 | MDL No. : | MFCD00006572 |
Formula : | C4H8O4 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | YLVACWCCJCZITJ-UHFFFAOYSA-N |
M.W : | 120.10 | Pubchem ID : | 96170 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
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* 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 |
---|---|---|
92% | In ethanol; at 20℃; for 28.0h; | 5-Bromo-3-chloro-1 ,2-diaminobenzene (4.6 g; 20 mmol; 1 eq.) is dissolved in EtOH (200 mL) and 2,3-dixydroxy-1 ,4-dioxane (2.5 g, 20 mmol; 1 eq.) is added. The mixture is stirred for 4 h at room temperature and a second portion of 2,3-dihydroxy-1 ,4-dioxane (1.3 g; 10 mmol; 0.5 eq.) is added. After stirring for 24 h at room temperature, the reaction mixture is concentrated and the residue is purified by FCC (EtOAc gradient in hexane) to provide 7- bromo-5-chloroquinoxaline as a beige solid (4.7 g; yield: 92%; UPLC purity: 98%). |
92% | In ethanol; at 20℃; for 28.0h; | 5-bromo-3-chloro-1 ,2-diaminobenzene (4.6 g; 20 mmol; 1 .0 eq.) was dissolved in EtOH (200 ml_) and then 2,3-dihydroxy-1 ,4-dioxane (2.5 g, 20 mmol; 1 .0 eq.) was added. The mixture was stirred for 4 h at RT and a second portion of 2,3-dihydroxy-1 ,4-dioxane (1 .3 g; 10 mmol; 0.5 eq.) was added. After stirring for 24 h at rt, RM was concentrated in a rotary evaporator and the residue was purified by FCC to provide 7-bromo-5- chloroquinoxaline (Intermediate 3) as a beige solid (4.7 g; yield 92 %; 98 % by UPLC). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96.7% | In N,N-dimethyl-formamide; at 90.0℃; for 8.0h; | Take a 100ml single-mouth bottle,Add 3,4-diaminobenzoic acid methyl ester (2) 3.32 g (0.02 mol),And added 30 ml of N,N-dimethylformamide, and dissolved by stirring.Then, [1,4]dioxane-2,3-diol (a) 3.6 g (0.03 mol) was added.Stir at 90 C for 8 hours.Then extracted, washed,Drying to give methyl quinoxaline-6-carboxylate (3)3.64 g, yield 96.7%. |