関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Mercaptoethanesulfonic acid | HCID 598 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Bromo-1-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethan-1-one | HCID 2801337 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1,1,4,4-Tetramethyltetralin | HCID 81186 | — |
| 生成物 | Sodium | HCID 5360545 | — |
反応手順
To a solution of 6-(bromoacetyl)-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene (12) (15.5 mg, 0.050 mmol) in DMF (0.13 mL) and THF (0.13 mL) was added a freshly prepared solution of 2-mercapto-1-ethanesulfonic acid, sodium salt (2) (25 mg, 0.15 mmol) and potassium carbonate (21 mg, 0.15 mmol) in water (0.15 mL) at room temperature. The resulting biphasic mixture was stirred for 30 min. The reaction mixture was diluted with ethyl acetate (2.5 mL), and the organic layer was separated, washed with water (2×1 mL) and brine (1×1 mL), dried and concentrated to afford 6-[2'-mercapto-1'-ethanesulfonic acid, sodium salt)acetyl]-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene (20) as a solid. 1H NMR (pyr-d5): δ 8.19, 7.90, 7.40 (m, 3H), 4.11 (s, 2H), 3.5 (m, 4H), 1.55 (s, 4H), 1.20 (d, 12H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05632898 |
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| 出典データセット | uspto-grants-1997_05 |
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| ORD ID | ord-bd07e98aceef4b509d4e39b6ba9624c9 |
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| 出典メモ | uspto-grants-1997_05 |
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