関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | [(4-(Allyloxylmethyl)phenyl)(phenyl)methylene]hydrazine | HCID 72240815 | — |
| 触媒 | Mercuric oxide | HCID 30856 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(Allyloxymethyl)-4-(diazo(phenyl)methyl)benzene | HCID 86639976 | 100% |
反応手順
To a mixture of mercury (II) oxide (3.1 g, 14 mmol), sodium sulphate (2.4 g, 16 mmol) and sat potassium hydroxide in ethanol (3 ml) was added a solution of 10 (3.2 g, 12 mmol) in dry TIM (20 ml). The mixture was stirred in the dark for 2 h. then filtered through a celite pad. Concentration of the filtrate in vacuo yielded 11 (3.1 g, 100%) as a dark red oil; δH (CDCl3) 3.90-3.94 (m, 2H, OCH2CH═CH2), 4.38 (s, 2H, ArCH2O), 5.05-5.26 (m, 2H, OCH2CH═CH2), 5.74-5.94 (m, 1H, OCH2CH═CH2), 7.12-7.36 (m, 9H, Ar—H) ppm; δC 71.0, 71.6 (OCH2CH═CH2, ArCH2O), 117.0 (OCH2CH═CH2), 124.9, 125.0, 125.4, 128.5, 129.0 (Ar—C), 129.8, 130.1 (1-, 1′-C), 134.5 (OCH2CH═CH2), 135.6 (4-C) ppm; νmax (thin film) 3029, 2855, 2038, 1596, 1512, 1494, 1085 cm−1; m/z (Fr) 264 ([M]+, 70%), 252 (100%), 196 (35%); found (Fr) 264.1250, C17H16N2O requires 264.1263.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08530212B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-f7b3d5c106f5425b877cc657efd6046a |
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| 出典メモ | uspto-grants-2013_09 |
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