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Potassium Phosphate, Tribasic → 6-Bromoimidazo[1,2-a]pyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | N-{6-bromoimidazo[1,2-a]pyridin-2-yl}-2,2,2-trifluoroacetamide | HCID 12065953 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 6-Bromoimidazo[1,2-a]pyridin-2-amine | HCID 44119296 | — |
反応手順
A stirred solution of N-(6-bromo-imidazo[1,2-a]pyridin-2-yl)-2,2,2-trifluoro-acetamide (9.0 g, 29.2 mmol) in DME (90 ml) and 1.27 M aqueous potassium phosphate (80.5 ml, 102.3 mmol) is heated at 90° C. overnight. After cooling to room temperature, the two layers are separate and the aqueous portion is extracted with EtOAc. The combined organic extracts are concentrated in vacuo to afford a brown oil. Iso-hexanes is added to the oil resulting in the formation of a solid. The excess iso-hexanes is decanted off and the remaining DME is azeotroped with THF (2×50 ml) to afford the title compound as a solid [MH+ 211.93].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08053574B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-09f3c55c328649578162ddb714c4b524 |
| 出典メモ | uspto-grants-2011_11 |