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CAS No. : | 16712-64-4 | MDL No. : | MFCD00060070 |
Formula : | C11H8O3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | KAUQJMHLAFIZDU-UHFFFAOYSA-N |
M.W : | 188.18 | Pubchem ID : | 85557 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H332-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 |
---|---|---|
In a reaction vessel equipped with a Dean-Stark apparatus and a condenser, 10.0 g of the compound represented by the formula (C-4-1)15.2 g of the compound represented by the formula (C-4-2), 0.8 g of phosphoric acid,150 mL of mesitylene was added,And heated under reflux for 20 hours while removing water.After cooling, the solid was filtered and dispersed and washed with water. And dried to obtain 21.8 g of a compound represented by the formula (C-4). Under a nitrogen atmosphere,2.0 g of the compound represented by the formula (C-4) produced in Example 1-7,4.0 g of the compound represented by formula (D-2-1)0.1 g of 4-dimethylaminopyridine,40 mL of dichloromethane was added.2.1 g of diisopropylcarbodiimide was added dropwise while cooling with ice, and the mixture was stirred at room temperature for 10 hours.The precipitate was removed by filtration, and the filtrate was washed successively with 1percent hydrochloric acid, water and brine.After recrystallization (dichloromethane / methanol), purification was carried out by column chromatography (silica gel, dichloromethane) and recrystallization (dichloromethane / methanol) to obtain 4.6 g of the compound represented by the formula (D-2) .The obtained compound had a purity of 98.644percent (impurity content represented by formula (C-4) of 0.006percent, impurity content represented by formula (F1-2) and formula (F2-2) 0.120percent). |