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Triphenylphosphine → ethyl (2Z)-2-(4-oxocyclohexyl)oxyimino-2-[2-(tritylamino)-1,3-thiazol-4-yl]acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Potassium Bromide | HCID 253877 | — |
| 反応物 | Azodicarboxylic acid dimethyl ester | HCID 351621 | — |
| 反応物 | 4-Hydroxycyclohexanone | HCID 543706 | — |
| 反応物 | (Z)-Ethyl 2-(hydroxyimino)-2-(2-(tritylamino)thiazol-4-yl)acetate | HCID 6410761 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | ethyl (2Z)-2-(4-oxocyclohexyl)oxyimino-2-[2-(tritylamino)-1,3-thiazol-4-yl]acetate | HCID 88627796 | — |
反応手順
4-Hydroxycyclohexanone (570 mg; J. B. Aldersley, G. N. Burkhardt, A. E. Gillam, and N. C. Hindley, J. Chem. Soc., 1940, 10) ethyl 2-(2-tritylaminothiazol-4-yl)-(Z)-2-hydroxyiminoacetate (1.37 g) and triphenyl-phosphine (860 mg) in anhydrous benzene (9 ml) were allowed to react with dimethyl azodicarboxylate (0.40 ml) as described in Example 67c except the reaction time was 14 days. Workup and chromatography gave the title compound (158 mg), νmax (KBr) 3390, 1737, 1710, 1596, 1585, 1529, and 1491cm-1 ; δH (CDCl3) 1.33 (3H, t, J 7Hz), 2.01, 2.31, and 2.55 (8H, 3m), 4.36 (2H, q, J 7z), 4.73 (1H, m), 6.52 (1H, s), 6.97 (1H, brs, D2O exch.), and 7.30 (15H, br s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04816452 |
| 出典データセット | uspto-grants-1989_03 |
| ORD ID | ord-b74806e46eb14c82a472f13ae452f449 |
| 出典メモ | uspto-grants-1989_03 |