関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyltrimethylammonium hydroxide | HCID 66854 | — |
| 反応物 | Methyl (methylsulfinyl)methyl sulfide | HCID 99129 | — |
| 反応物 | 2,6-Dimethylbenzaldehyde | HCID 583841 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-(2-Methanesulfinyl-2-methylsulfanyl-vinyl)-1,3-dimethyl-benzene | HCID 86631265 | 68.3% |
反応手順
To a solution of 2,6-dimethyl-benzaldehyde (14.6 g, 109 mmol) in 1,4-dioxane (24.7 mL) was added methyl methylsulfinylmethyl sulfide (13.5 g, 109 mmol) followed by benzyltrimethylammonium hydroxide (9.10 g, 54.4 mmol). The resulting mixture was heated at 80° C. After 16 h, the mixture was cooled to rt and concentrated. The resulting residue was purified by FCC to afford a yellow oil (17.9 g, 68%). MS (ESI): mass calcd. for C12H16OS2, 240.1; m/z found, 241.1 [M+H]+. 1H NMR (CDCl3): 7.71 (s, 1H), 7.19-7.13 (m, 1H), 7.07 (d, J=7.5 Hz, 2H), 2.82 (s, 3H), 2.24 (s, 6H), 2.06 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09440978B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-4f5865c9b645451dbc571947ad8f366c |
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| 出典メモ | uspto-grants-2016_09 |
|---|
