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Water → 2-Chloro-6-(2,4-difluoro-phenoxy)-quinazoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tert-Butyl nitrite | HCID 10906 | — |
| 反応物 | 2-Chloro-6-(2,4-difluoro-phenoxy)-quinazolin-4-ylamine | HCID 58905130 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Chloro-6-(2,4-difluoro-phenoxy)-quinazoline | HCID 58905137 | 44.2% |
反応手順
Compound (1G) (21 g, 0.07 mol) was dissolved in THF (200 mL) and the solution added dropwise to a solution of t-butyl nitrite (16.5 mL, 0.14 mol) in THF (100 mL). The mixture was heated to reflux for 4 h, and after cooling to room temperature, the reaction mixture was poured into water and extracted with EtOAc (2×100 mL). The combined organic layers were dried over sodium sulfate and evaporated in vacuo. The crude product was purified by chromatography (silica gel, hexane: EtOAc, 4:1) giving 9.05 g of 2-chloro-6-(2,4-difluoro-phenoxy)-quinazoline (1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07456185B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-a11f365f54df4e5f90ccbf118752ef52 |
| 出典メモ | uspto-grants-2008_11 |