関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethyl phosphite | HCID 31215 | — |
| 反応物 | 3,5-Difluorobenzyl bromide | HCID 518896 | — |
| 生成物 | (3,5-Difluoro-benzyl)-phosphonic acid diethyl ester | HCID 11219261 | — |
反応手順
3,5-difluorobenzyl bromide (3.0 mL, 23.2 mmol) was combined with triethylphosphite (9.1 mL, 53.3 mmol) and the mixture heated and stirred at 135° C. overnight. The mixture was put under hi-vacuum and heated to 70° C. for 12 hours. The final product was a clear oil (5.78 g, 94% yield). 1H NMR (400.14 MHz, CDCl3) δ 6.83 (m, 2H), 6.71 (dt, J=9.00, 2.28 Hz), 4.06 (m, 4H), 3.12 (d, J=21.94 Hz, 2H), 1.28 (t, J=7.09 Hz, 6H). 31P{1H} NMR (161.97 MHz, CDCl3): δ 25.22.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08586208B2 |
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| 出典データセット | uspto-grants-2013_11 |
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| ORD ID | ord-e75abd61a99e4fd0b9e561d54f43090c |
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| 出典メモ | uspto-grants-2013_11 |
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