関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromocyclopentane | HCID 8728 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-(Hydroxymethyl)-2-nitrophenol | HCID 14520114 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Cyclopentoxy-4-nitrobenzyl alcohol | HCID 54346795 | — |
反応手順
To a solution of 9.6 g (56.5 mmol) of 3-hydroxy-4-nitrobenzyl alcohol in 960 mL of dry N,N-dimethylformamide under a nitrogen atmosphere was added 11.7 g (83.6 mmol) of anhydrous potassium carbonate followed by 18.1 mL (169.0 mmol) of cyclopentyl bromide. The reaction mixture was warmed to 50° C. for 24 hours after which time the mixture was cooled to room temperature and concentrated to a dark brown residue under high vacuum. The residue was dissolved in 500 mL of chloroform, washed with two, 50 mL portions of saturated sodium chloride, dried over magnesium sulfate, and concentrated to dryness. Purification of the crude product with liquid chromatography over 200 g of silica gel and eluting with 10% methanol in chloroform provided the analytically pure 3-cyclopentoxy-4-nitrobenzyl alcohol upon drying in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05274002 |
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| 出典データセット | uspto-grants-1993_12 |
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| ORD ID | ord-8b34d301ec5f4aee878efd87a67d8f23 |
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| 出典メモ | uspto-grants-1993_12 |
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