関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Bromo-6-fluoropyridine | HCID 639438 | — |
| 反応物 | (2,2-Difluorocyclopropyl)methanol | HCID 2761401 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-Bromo-6-(2,2-difluoro-cyclopropylmethoxy)-pyridine | HCID 86689014 | — |
反応手順
To 307 mg (2.84 mmol) (2,2-difluorocyclopropyl)methanol in 1,4-dioxane (10 mL) is added 69 mg (2.84 mmol) sodium hydride and 500 mg (2.84 mmol) 2-bromo-6-fluoropyridine. The mixture is stirred for 2 h at 90° C. Water and DMF are added and the mixture is filtered and concentrated in vacuo. The residue is purified by HPLC (C18 RP Sunfire, acetonitrile/water (+0.1% TFA)) to yield the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08530461B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-8d611a51858c41169343e7666344cf94 |
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| 出典メモ | uspto-grants-2013_09 |
|---|
