化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → Acetic acid 2-ethyl-3-oxo-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 2-Ethyl-3-oxobutanol | HCID 270299 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Acetic acid 2-ethyl-3-oxo-butyl ester | HCID 10898964 | — |
反応手順
3-Hydroxymethyl-pentan-2-one (20.7 g) was dissolved in CHCl3 (150 mL) and cooled in an ice bath. Acetic anhydride (80 mL) was added, followed by DMAP (2.18 g), and the mixture was stirred overnight at room temperature. After cooling in an ice bath, MeOH (120 mL) was added dropwise, and the mixture was poured into a saturated aqueous NaHCO3 solution. After extraction with DCM twice, the combined organic phases were dried over Na2SO4 and evaporated under reduced pressure to give 28.0 g of a light-yellow liquid. 1H NMR (400 MHz, CDCl3) δ 0.93 (t, J=8 Hz, 3H), 1.46-1.75 (m, 2H), 2.03 (s, 3H), 2.20 (s, 3H), 2.77 (quint., J=6.5 Hz, 1H), 4.20 (d, J=7 Hz, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728018B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-59cd7a8427e64aa59ace39ad6c78da57 |
| 出典メモ | uspto-grants-2010_06 |