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Triethylamine → Phenethylisoselenocyanate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | Formamide, N-(2-phenylethyl)- | HCID 140995 | — |
| 反応物 | Selenium | HCID 6326970 | — |
| 反応物 | Benzyl Isoselenocyanate | HCID 12506035 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Phenethylisoselenocyanate | HCID 25060470 | 95% |
反応手順
(AS3.091) A mixture of phenylethylformamide (g, 1.5 mmol), triethylamine (6.4 mmol), 4 Å molecular sieves (g), triphosgene (0.8 mmol), and selenium powder (3.0 mmol) in CH2Cl2 was refluxed and worked up as mentioned for 2a. The crude residue thus obtained was purified by silica gel column chromatography (EtOAc/hexanes 2:98) to give 0.96 g (95%) of 2b as an oil. 1H NMR (CDCl3) δ 3.03 (t, 2H, J=6.9 Hz), 3.81 (t, 2H, J=6.9 Hz) 7.20-7.38 (m, 5H); HRMS (EI) calcd for C9H9NSe, 210.9895. found, 210.9892.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09096505B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-45b41c2d14c144e5bf8cbaf74e340921 |
| 出典メモ | uspto-grants-2015_08 |