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Triphenylphosphine → HCID 117729706、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 1-Morpholinoethanol | HCID 3029376 | — |
| 反応物 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 反応物 | 5-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)-2-chlorophenol | HCID 68952645 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 117729706 | HCID 117729706 | 80% |
反応手順
To a stirred solution of 5-(5-amino-3-tert-butyl-pyrazol-1-yl)-2-chloro-phenol (WO2007/091152, which is incorporated herein by reference; 200 mg, 0.75 mmol), 2-N morpholino ethanol (137 μL, 1.13 mmol) and Ph3P (394 mg, 1.50 mmol) in THF (7.5 mL) at 0° C. was added DEAD (236 μL, 1.50 mmol). After 1 h, the reaction mixture was diluted with water and extracted with DCM. The combined organics were dried and concentrated in vacuo. The residue was purified by FCC, using 0-5% [2M NH3 in MeOH] in DCM, to give the title compound (228 mg, 80%). LCMS (Method 3): Rt 2.28 min, m/z 379 [MH+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440974B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-a8c53b9729bd4bf6ae02d50abae60ae2 |
| 出典メモ | uspto-grants-2016_09 |