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N-Iodosuccinimide → HCID 131723500、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 反応物 | Dibenzylphosphate | HCID 4193600 | — |
| 反応物 | (Methylsulfanyl)[(methylsulfanyl)methoxy]methane | HCID 21902172 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 131723500 | HCID 131723500 | 94.9% |
反応手順
To a solution of bis(methylthiomethyl)ether (30 mg, 2.34 mmol) and molecular sieves (300 mg) in THF (100 ml) at room temperature was added dibenzyl phosphate (2.74 g, 9.85 mmol) followed by N-iodosuccinimide (608 mg, 2.71 mmol) and the solution was stirred for 4 h. The reaction mixture was then diluted with ethyl acetate and filtered through a pad of celite. The filtrate was treated with a 1:1 (v:v) solution of saturated aqueous sodium bicarbonate and 5% aqueous sodium thiosulfate. The colorless organic extract was then washed with brine, dried over sodium sulfate and concentrated in vacuo to provide 600 mg (69%) of the title compound:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06455575B2 |
| 出典データセット | uspto-grants-2002_09 |
| ORD ID | ord-3055ee1053f64d82a480eaa4622c6a1f |
| 出典メモ | uspto-grants-2002_09 |