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Acetic Acid → (6-Methoxy-3-nitro-2-pyridinyl)methyl phenyl sulfone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2-Methoxy-5-nitropyridine | HCID 79525 | — |
| 反応物 | ((Chloromethyl)sulphonyl)benzene | HCID 81625 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (6-Methoxy-3-nitro-2-pyridinyl)methyl phenyl sulfone | HCID 13902761 | 80% |
反応手順
A 1 M KOt-Bu solution in tetrahydrofuran (50 mL, 50 mmol) is cooled to −40° C., treated portion-wise with a solution of chloromethyl phenyl sulfone (4.39 g, 23.0 mmol) and then with a solution of 2-methoxy-5-nitropyridine (3.55 g, 23.0 mmol) in tetrahydrofuran, stirred for 45 min at −40° C., treated with glacial acetic acid (3.0 g, 50 mmol) and filtered. The filtercake is air-dried to give the title compound as a tan solid, 5.70 g (80% yield), mp 147-149° C., identified by mass spectral and HNMR analyses.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07585873B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-96090cd68d904704b46e3ea011558c57 |
| 出典メモ | uspto-grants-2009_09 |