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Sulphenone → Hydrazine, (4-(phenylsulfonyl)phenyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulphenone | HCID 6621 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 触媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Hydrazine, (4-(phenylsulfonyl)phenyl)- | HCID 116834 | — |
反応手順
A mixture of 4-chlorophenyl phenyl sulfone (10.1 g, 40.0 mmol), hydrazine mono-hydrate (30 mL), and triethylamine (4 drops) in ethylene glycol (20 mL) is heated at 150° for 15 hr. Upon cooling, the mixture is diluted with H2O and filtered. The residual solid is washed with H2O until the washings are neural (pH=6). This material is then triturated with methylene chloride and dried under reduced pressure at 50° to give the title compound, IR (drift) 3282, 1586, 1514, 1306, 1291, 1158, 1145, 1104, 996, 813, 756, 730, 717, 688 and 678 cm−1; NMR (300 MHz, CDCl3) 7.70-7.85, 7.45-7.65, 6.79 and 4.22 δ; MS (EI) m/z 248 (M+), 125, 123, 108, 107, 90, 80, 77, 63 and 51.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06921823B2 |
| 出典データセット | uspto-grants-2005_07 |
| ORD ID | ord-65af31b2ddd44f9e9e85be1f805ae758 |
| 出典メモ | uspto-grants-2005_07 |