関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Cyclobutanol | HCID 76218 | — |
| 反応物 | 5-Bromo-2-chloropyrimidine | HCID 606665 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-Bromo-2-cyclobutoxypyrimidine | HCID 49758704 | — |
反応手順
2.42 mL (31.0 mmol) cyclobutanol and 3.00 g (15.5 mmol) 5-bromo-2-chloropyrimidine are added to 40 mL 1,4-dioxane and cooled down to 0° C. Then the reaction mixture is charged with 1.86 g (46.5 mmol) NaH. After removing of the cooling bath the reaction mixture is stirred at r.t. for 1 h. The reaction is quenched by the addition of water and sat. aq. NaHCO3 solution. The 1,4-dioxane is removed in vacuo and the aq. residue is extracted with DCM. The org. phases are combined, washed with water and dried with MgSO4. The solvent is removed under reduced pressure. The crude product is used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08530460B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-8f31d6a655944a2e8d985c997c38e401 |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|