関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Benzyl bromoacetate | HCID 62576 | — |
| 反応物 | Benzyl [(1S)-2-(7-formyl-6-hydroxy-1H-indazol-1-yl)-1-methylethyl]carbamate | HCID 136385114 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 68856363 | HCID 68856363 | 71.1% |
反応手順
To a stirred solution of the product from Step C, Example 1 (0.12 g, 0.32 mmol) in DMF (10 mL) was added potassium carbonate (0.15 g, 1.05 mmol) followed by benzyl 2-bromoacetate (0.08 g, 0.48 mmol) at room temperature and the mixture was heated at 70° C. for 20 h. A saturated aqueous solution of ammonium chloride (20 mL) was added followed by ethyl acetate (50 mL). The organic layer was separated and the aqueous was extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine (30 mL), dried and evaporated to a residue, which was purified by chromatography (silica, 50% ethyl acetate in hexane) to give a solid (0.11 g, 71%): mp 140-141° C.; MS (ES) m/z 484 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07476687B2 |
|---|
| 出典データセット | uspto-grants-2009_01 |
|---|
| ORD ID | ord-bf1daf8d1fac4e24b0f33a502006a7a1 |
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| 出典メモ | uspto-grants-2009_01 |
|---|
