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Acetyl chloride → p-Acetamidophenyl methyl disulfide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | p-Aminophenyl methyl disulfide | HCID 25001884 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | p-Acetamidophenyl methyl disulfide | HCID 24997137 | — |
反応手順
To a solution of 39a (50 mg, 0.3 mmol) in dry CH2Cl2 (3 ml) was added triethylamine (127 μL, 0.9 mmol, 3 eq.), followed by acetyl chloride (32 μL, 0.45 mmol). The reaction was stirred at RT for 1 hr., then was diluted with dichloromethane, washed with water, then 5% aq. HCl, then 5% aq. NaHCO3. Dried over MgSO4, then concentrated in vacuo to give a yellow oil which solidified on standing. Chromotography (1:1 petroleum ether:ethyl acetate) gave 18 mg (29%) as a light brown solid. 1H NMR (400 MHz, CDCl3): δ 7.47 (s, 4H); 2.41 (s, 3H); 2.16 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08722937B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-02865d9f5c6c4fc39296565f96c43ef5 |
| 出典メモ | uspto-grants-2014_05 |