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Hydrochloric Acid → {[5-(1-Methyl-1-hydroxyethyl)isoxazol-3-yl]methyl}malononitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | {[5-(1-Hydroxy-1-methylethyl)-isoxazol-3-yl]methylidene}malononitrile | HCID 57736335 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | {[5-(1-Methyl-1-hydroxyethyl)isoxazol-3-yl]methyl}malononitrile | HCID 57736354 | 53.8% |
反応手順
9.91 g of {[5-(1-hydroxy-1-methylethyl)-isoxazol-3-yl]methylidene}malononitrile was dissolved in 100 ml of tetrahydrofuran, and 3.78 g of sodium borohydride was then added under ice-cooling. The mixture was stirred for 8 hours under ice-cooling. The reaction mixture was added to 0.5 N hydrochloric acid over 30 minutes and then extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 5.38 g of {[5-(1-hydroxy-1-methylethyl)-isoxazol-3-yl]methyl}malononitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07846956B2 |
| 出典データセット | uspto-grants-2010_12 |
| ORD ID | ord-c381e5a3887b48ce80b4ef37c5f71cd9 |
| 出典メモ | uspto-grants-2010_12 |