関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Zopiclone | HCID 5735 | — |
| 反応物 | Benzenesulfonic Acid | HCID 7371 | — |
| 反応物 | Eszopiclone | HCID 969472 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (S)-Zopiclone Besylate | HCID 131729769 | 92.7% |
反応手順
A 2000 mL reactor was charged with 10.0 g (S)-zopiclone and 400 mL tetrahydrofuran (THF). The contents were heated to 35° C. Into a 1000 mL reactor was charged 4.4 g benzenesulfonic acid and 400 mL THF, and stirred until a solution was formed. The acid solution was transferred slowly to the zopiclone solution. The reaction was cooled to 15° C. and stirred for 18 hr at 20-25° C. The reactor slurry was filtered and washed with THF in an appropriate filter. The wet cake was dried under vacuum at 60-65° C. and packaged in an appropriate container. Isolated yield=92.7%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08497267B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-bfe88e8f1e17489882f240f8f4f9daaf |
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| 出典メモ | uspto-grants-2013_07 |
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