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CAS No. : | 390427-07-3 | MDL No. : | MFCD11655886 |
Formula : | C12H17NO3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | SAIZFIRMLDAPKH-UHFFFAOYSA-N |
M.W : | 223.27 | Pubchem ID : | 12074946 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-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 |
---|---|---|
67.07% | Reflux; | The compound of formula 2 (10.0g),Glacial acetic acid (50.0mL) was added to the reaction flask and stirred,Stop the reaction after refluxing for 6h7h,Cool down to below 20,Slowly add MTBE (150mL) to crystallize,Stir at 1020 for 0.5h, filter,Dry under vacuum at 40 to constant weight;Weight: 5.50g; Yield: 67.07%;Purity: 98.64%. |
42 g | Methanol (350 ml) and the crude product (1.00 eq) obtained in Example 1 were added to a 1 L reaction flask at 15-30 C, and water (50 ml L) and concentrated hydrochloric acid (100 ml, 2.00 eq) were added to a 1 L reaction flask.After stirring at 15-30 C for 16 hours, the sample was detected by HPLC to <0.5% of the starting material.After the reaction, the system is concentrated to remove methanol, and 500 ml of water is added to the concentrated system to form a solution.The phase is then extracted with ethyl acetate (350 ml * 2), the aqueous phase is extracted after the extraction, the pH is adjusted to 7-8 by adding 85 g of sodium hydrogencarbonate, and the mixture is extracted with 2-methyltetrahydrofuran 4 times, 700 ml each time;The organic phase is concentrated to dryness to give a yellow solid;Soluble in 350ml acetic acid,Stir at 16-30 C for 16 hrs.Add 1000 ml of methyl tert-butyl ether to the system.Solid precipitated, stirred at 15-30 C for 1-2hrs; suction filtration,The filter cake was rinsed with methyl tert-butyl ether; the product was dried to give 42 g. |