HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Benzyl-1H-pyrazol-5-amine → 1-benzyl-N-(4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-1H-pyrazol-5-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Benzyl-1H-pyrazol-5-amine | HCID 77061 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | 4-(tert-Butyldimethylsilyloxy)cyclohexanone | HCID 10609430 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 1-benzyl-N-(4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-1H-pyrazol-5-amine | HCID 67008644 | 9.1% |
Reaction Steps
To a solution of 1-benzyl-1H-pyrazol-5-amine (6.3 g) in acetic acid (70 mL) was added 4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexanone (10 g) and the mixture was stirred for 30 min. After stirring, sodium triacetoxyborohydride (12.0 g) was added, and the mixture was stirred for 18 hr. Acetic acid was evaporated and ethyl acetate and water were added to the residue. The mixture was neutralized with sodium hydrogen carbonate, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography to give the title compound as a pale-yellow amorphous solid (1.27 g, 9%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115136B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-6b2a7293bee640519e3b9dd78332a380 |
| Source note | uspto-grants-2015_08 |