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Diethyl Ether → 1,3-Benzodithiolylium Tetrafluoroborate (Hydroxyl-Protecting Agent)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 1,3-Dithiaindane, 2-(3-methylbutyl)oxy- | HCID 592641 | — |
| 反応物 | Trifluoroborane Hydrofluoride | HCID 9855450 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 1,3-Benzodithiolylium Tetrafluoroborate (Hydroxyl-Protecting Agent) | HCID 2735971 | 50% |
反応手順
16.0 g (0.067 mole) of 2-isopentyloxy-1,3-benzodithiol (V) obtained in Synthesis Example 1 was dissolved in 200 ml of acetic anhydride. A 42% aqueous solution of hydrofluoroboric acid was added dropwise to the reaction solution in 30 minutes under cooling with ice. After the reaction solution was stirred at room temperature for 30 minutes, 200 ml of diethyl ether was added thereto. The formed salt was filtered off and washed with 100 ml of diethyl ether. The resulting salt was dried to obtain 12.0 g (yield: 50%) of the desired compound (VI) as a white crystal (decomposition temperature: 150°-151° C.). The physical properties of the compound were as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05229238 |
| 出典データセット | uspto-grants-1993_07 |
| ORD ID | ord-d6f4a5e010db430e8eea160dd93b63d8 |
| 出典メモ | uspto-grants-1993_07 |