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CAS No. : | 28539-02-8 | MDL No. : | MFCD00179118 |
Formula : | C7H7N3O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MXJIHEXYGRXHGP-UHFFFAOYSA-N |
M.W : | 149.15 | Pubchem ID : | 224169 |
Synonyms : |
|
Chemical Name : | 1-(Hydroxymethyl)benzotriazole |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
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 |
---|---|---|
22% | With hydrogenchloride; sodium tetrahydroborate; In 1,4-dioxane; ethanol; water; | To <strong>[180683-64-1]tert-butyl ((1S,2S)-2-aminocyclohexyl)carbamate</strong> (17-1, 1.00 g, 4.67 mmol), (1H-benzo[d][1,2,3]triazol-1-yl)methanol (17-2, 0.696 g, 4.67 mmol) and 4M HCl in dioxane (1.17 mL, 4.67 mmol) in EtOH (30 mL) was added sodium borohydride (0.353 g, 9.33 mmol) and the resulting mixture was stirred overnight. The reaction mixture was concentrated and the resulting residue was purified by reverse phase RP-C18 column chromatography eluting with 5 to 60% MeCN in water to provide 17-3 (230 mg, 1.03 mmol, 22% yield) as a white solid. 1H NMR (400 MHz, methylene chloride-d2) 6 4.85-4.39 (m, 1H), 3.26-2.87 (m, 1H), 2.27 (s, 3H), 2.13-1.92 (m, 3H), 1.68-1.54 (m, 2H), 1.34 (s, 9H), 1.25-0.92 (m, 4H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
44% | To <strong>[180683-64-1]tert-butyl ((1S,2S)-2-aminocyclohexyl)carbamate</strong> (17-1, 500 mg, 2.33 mmol) in EtOH (30 mL) was added (1H-benzo[d][1,2,3]triazol-1-yl)methanol (17-2, 750 mg, 4.67 mmol) and the resulting mixture was stirred for 3 h. Sodium borohydride (265 mg, 7.00 mmol) was then added and stirring was continued overnight. The reaction mixture was concentrated and then quenched with water. The aqueous phase was extracted with DCM (*3) and the combined organic phases were dried over Na2SO4, filtered, and concentrated. The crude residue was purified by reverse phase RP-C18 column chromatography column eluting with 10 to 100% MeCN in water with 0.1% NH4OH as a modifier to provide the product 25-1 (250 mg, 1.03 mmol, 44% yield) as a white solid. MS [M+H]+=243.2. |
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