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CAS No. : | 39124-19-1 | MDL No. : | MFCD01710740 |
Formula : | C7H10N2O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 170.17 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* 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 |
---|---|---|
82% | Stage #1: for 48 h; Reflux Stage #2: With sodium hydroxide In 1,4-dioxane; methanol; water at 20℃; for 15 h; |
[Step 2] Synthesis of 4-((tert-butoxycarbonyl)amino)tetrahydro-2H-pyran-4-carboxylic acid: Calcium hydroxide (3.0 g, 41 mmol) was added to an aqueous solution (30 mL) of Reference Example Compound 31 (2.2 g, 13 mmol) at room temperature. The resulting reaction solution was heated to reflux for 48 hours with stirring, and then filtered through Celite, followed by washing of the filtered product with hot water. The filtrate was concentrated under reduced pressure, and the obtained crude product was dissolved in a mixture of water, 1,4-dioxane and methanol (water: 1,4-dioxane:methanol = 10:10:3, 23 mL). Di-tert-butyldicarbonate (3.4 g, 16 mmol) and sodium hydroxide (0.50 g, 13 mmol) were added to the reaction solution at room temperature. The reaction solution was stirred at room temperature for 15 hours, and then concentrated under reduced pressure. Dilute hydrochloric acid (15 mL) was added to the obtained crude product, and extraction was performed with a mixture of chloroform and methanol (chloroform:methanol = 10:1). The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure, to obtain 2.6 g (82percent) of 4-((tert-butoxycarbonyl)amino)tetrahydro-2H-pyran-4-carboxylic acid (hereinafter referred to as Reference Example Compound 32). |