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
In a reaction similar to Example 1a, about 30.0 grams of sevoflurane (0.15 mols) was placed in a 250-mL 3-neck flask under nitrogen, and cooled in a dry ice-acetone bath to about −0.1° C. Approximately 50 mL of a 3.0 M solution of CH3Li/CH2(OC2H5)2 (0.15 mols of the base) was added to the sevoflurane over about 2 hours and 38 minutes while maintaining a reaction temperature between about −8° C. and about +9° C. A violent, exothermic reaction was observed. The reaction mixture was then stirred at about −2° C. to about +6° C. for an additional 30 minutes. A vacuum (3.3 mm Hg) applied to the reaction mixture for approximately 2 hours, 17 minutes while the reaction mixture was held at a temperature between about −30° C. and about −17° C. yielded about 17.9 grams of a crude liquid product. The crude liquid contained 17.9% sevoflurane compound A, 70.6% CH2(OC2H5)2, and other side products.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09353038B2 |
|---|
| 出典データセット | uspto-grants-2016_05 |
|---|
| ORD ID | ord-e9524eb896e747c08e5050cf1d3a753c |
|---|
| 出典メモ | uspto-grants-2016_05 |
|---|