関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | (1R,4R)-1,4-bis(4-nitrophenyl)butane-1,4-diol | HCID 59616924 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,4-Bis(4-nitrophenyl)butane-1,4-diyl dimethanesulfonate | HCID 59617179 | 64% |
反応手順
To a solution of the product from Example 1B (0.80 g, 2.407 mmol) in dry CH2Cl2 (25 ml) at 0° C. was added triethylamine (1.007 ml, 7.22 mmol), followed by dropwise addition of methanesulfonyl chloride (0.469 ml, 6.02 mmol). The resulting mixture was stirred at 0° C. for 30 min, during which time the starting material slowly went into solution. After stirring an additional 1 h at 0° C., a precipitate began to form. Saturated aq NH4Cl (4 ml) was added, and stirring was continued at room temperature for 20 min. The mixture was washed with water (2×10 ml), and the organic layer was treated with hexanes (10 ml) to give an orange solid that was collected by filtration to give the title compound (0.75 gm, 64% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09006387B2 |
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| 出典データセット | uspto-grants-2015_04 |
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| ORD ID | ord-0b7f4742e0344cf98d52f500251aa39a |
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| 出典メモ | uspto-grants-2015_04 |
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