関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | (2-Methoxy-5-(2-methyl-2H-tetrazol-5-yl)phenyl)methanol | HCID 58993522 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-(3-(Bromomethyl)-4-methoxyphenyl)-2-methyl-2H-tetrazole | HCID 58993604 | 63% |
反応手順
(2-Methoxy-5-(2-methyl-2H-tetrazol-5-yl)phenyl)methanol (100 mg, 0.45 mmol) and triphenylphosphine (238 mg, 0.9 mmol) were combined in methylene chloride (3 mL) and cooled to 0° C. N-Bromosuccinimide (170 mg, 0.95 mmol) was introduced in portions and the reaction allowed to warm to room temperature. After 16 h, the reaction mixture was diluted with methylene chloride and washed with concentrated sodium bicarbonate (2×), brine (2×), dried over sodium sulfate, and concentrated. Column chromatography on silica gel (30% ethyl acetate/hexanes) gave 80 mg (63%) of the desired material. LC/MS (HPLC method 3): tR=2.69 min, 285.02 (MH)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08383821B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-0f6ed860ca1e454aaf44da6b9e398fa5 |
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| 出典メモ | uspto-grants-2013_02 |
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