関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Lutidine | HCID 7937 | — |
| 反応物 | tert-Butyldimethylsilyl trifluoromethanesulphonate | HCID 123564 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (5-Bromo-3-pyridinyl)methanol | HCID 2784733 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Bromo-5-(((tert-butyldimethylsilyl)oxy)methyl)pyridine | HCID 21984091 | — |
反応手順
Tert-butyldimethylsilyl trifluoromethanesulfonate (1.174 ml, 5.11 mmol) was added to 2,6-lutidine (0.743 ml, 6.38 mmol) and (5-bromopyridin-3-yl)methanol (800 mg, 4.25 mmol) stirred in CH2Cl2 (10 ml) cooled to 0° C. and the mixture was stirred at 0° C. for 1 h. Saturated aqueous sodium hydrogen carbonate was added to the reaction mixture and the mixture was extracted with ethyl acetate. The combined organic fractions were dried (Na2SO4), filtered and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography to provide 3-bromo-5-({[tertbutyl(dimethyl)silyl]oxy}methyl)pyridine: MS: cal'd 325 (MNa+), exp 325 (MNa+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07981874B2 |
|---|
| 出典データセット | uspto-grants-2011_07 |
|---|
| ORD ID | ord-ff87c445d7e44a4fb060c83b735553f1 |
|---|
| 出典メモ | uspto-grants-2011_07 |
|---|
