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Cesium carbonate → HCID 69231272、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,3-Diiodopropane | HCID 12314 | — |
| 反応物 | Methanesulfonylacetic acid methyl ester | HCID 2759918 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 69231272 | HCID 69231272 | 79% |
反応手順
To a solution of methyl methylsulfonylacetate (1.0 g, 6.6 mmol) in 20 mL of acetonitrile was added 1,3-diiodopropane (2.3 mL, 20 mmol) and cesium carbonate (6.4 g, 20 mmol). After stirring at room temperature for 2 h, the reaction was partitioned between water (50 mL) and ethyl acetate (100 mL). The organic layer was separated, dried over anhydrous magnesium sulfate, filtered and concentrated to dryness, and the residue was purified by flash chromatography on silica gel eluting with 20 to 50% ethyl acetate in hexane to give methyl 1-methylsulfonylcyclobutanecarboxlate (1.0 g, 79%). δ 3.84 (s, 3H), 3.02 (s, 3H), 2.84-2.65 (m, 4H), 2.25-2.02 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07423067B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-c4ab329b32dc4ec78c61c1605479c0ea |
| 出典メモ | uspto-grants-2008_09 |