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CAS No. : | 407623-72-7 | MDL No. : | MFCD04035600 |
Formula : | C11H16N2O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | FNGDRRWCPLWUDZ-UHFFFAOYSA-N |
M.W : | 224.26 | Pubchem ID : | 29920835 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P264-P271-P280-P302+P352-P304+P340-P305+P351+P338-P312-P362-P403+P233-P501 | UN#: | |
Hazard Statements: | 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 |
---|---|---|
In dichloromethane; at 20℃; for 1.0h; | To a solution of 4-aminopyridme-3-methanol (3) (Alfa Aesar) (806 mg. 6.5 mmol) in ( I LCh (10 mL) a solution of di-tert-butyl-dicarbonate (1.43 g, 6.56 mmol) in Ci hC 'h (5 mL) was added and stirred at room temperature for 1 h (TLC), After 1 h, the solution was acidified with 1 N HQ (7.4 mL, 7.4 mmol). The phases were separated and the aqueous phase was washed with CH2CI2. The aqueous layer was mixed with a fresh portion of CH2CI2 (10 mL) and treated with K2CO3 (71 1 mg, 5.1 mmol). The phases were separated and treated with additional amounts of CH2G2.. The combined organic extracts were dried (MgS04) and evaporated in vacuo to give a 60:40 mixture containing desired product 8 and the O-linked carbonate. Attempts to purify the N-carbamate by flash chromatography from the O- carbonate were unsuccessful due interconversion between these two species in solution at room temperature. -N ViR (CDC13, 500 MHz) delta: 1.53 (91 L s), 4.67 (2H, s), 4.83 (2H, br s), 7.95 ( i i . s), 8.07 (1H, d, ./ 5.5 Hz), 8.28 (I H, d, J ------ 5.5 Hz), 8.48 (1 H, s). This product has been previously synthesized through a different route (Mochizuki, et al, 2011). |