関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sevoflurane | HCID 5206 | — |
| 反応物 | Diethoxymethane | HCID 10024 | — |
| 生成物 | 1,1,3,3,3-Pentafluoro-2-(fluoromethoxy)-1-propene | HCID 105015 | — |
反応手順
30 grams of sevoflurane (0.15 mols) was cooled to about −36.2° C. under nitrogen. Approximately 10 mL of a 3.0 M solution of CH3Li/CH2(OC2H5)2 (0.03 mols of the base) was added over 29 minutes while maintaining a temperature between about −37.5° C. and about −30.5° C. After addition of the methyl lithium was complete, the addition funnel was washed with a few mL of diethoxymethane. The reaction mixture was then stirred for approximately 20 minutes at a temperature between about −39° C. and about −35° C. A vacuum (0.3 mmHg) applied to the reaction mixture for approximately 1 hour, 46 minutes while the reaction mixture was held at a temperature between about −38.5° C. and about 10.7° C. afforded approximately 30.0 grams of a crude liquid product. GC analysis of this liquid showed it contained 22.8% compound A, 47.1% unreacted sevoflurane, and 29.7% diethoxymethane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09353038B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-d7180bfd1f1d41e285eb71f3b18d58b5 |
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| 出典メモ | uspto-grants-2016_05 |
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