HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromo-2,2-dimethylpropane → HCID 70873072, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromo-2,2-dimethylpropane | HCID 12415 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178516021 | HCID 178516021 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 70873072 | HCID 70873072 | — |
Reaction Steps
To a solution of 6-(trifluoromethyl)pyridin-2-ol (5.00 g, 30.7 mmol) in dry DMF (50 mL) was added NaH (3.71 g, 92.1 mmol) under N2 and the mixture was stirred at rt for 1 h. Then 1-bromo-2,2-dimethylpropane (11.6 g, 76.7 mmol) was added and the resulting mixture was heated at 100° C. overnight, cooled, quenched with water (10 mL) and extracted with EA twice. The combined organic layers were washed with brine (3×), concentrated and purified by CC on NH silica gel (PE/EA=100/1) to give compound P12a (1.05 g, 15%) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946446B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-33f75df8f848436e861234748df7fcdf |
| Source note | uspto-grants-2015_02 |