関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 2-chloropropionate | HCID 10807 | — |
| 反応物 | Sodium methanesulfinate | HCID 2733271 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 2-(methylsulfonyl)propanoate | HCID 10511577 | 73% |
反応手順
Sodium methyl sulfinate (103 g, 937 mmol) was combined with the ethyl 2-chloropropionate (109 g, 892 mmol) in ethanol (350 mL) in a 500 mL one neck round bottom flask. The reaction was heated to 77° C. for 20 h, and then allowed to cool to room temperature. Solids were removed by filtration through celite, and the filter pad was washed with ethanol. The combined filtrates were concentrated under reduced pressure. The crude product was suspended in diethyl ether (250 mL), and solids were removed by filtration. The filtrate was concentrated under reduced pressure to afford the title compound as a pale yellow oil (51 g, 73%). 1H NMR (400 MHz, CHLOROFORM-d) δ1.32 (t, J=7.05 Hz, 3H) 1.67 (d, J=7.47 Hz, 3H) 3.05 (s, 3H) 3.83-3.92 (m, 1H) 4.18-4.37 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08748466B2 |
|---|
| 出典データセット | uspto-grants-2014_06 |
|---|
| ORD ID | ord-5d79a1cecebb4c3a8ba91f76b9533d09 |
|---|
| 出典メモ | uspto-grants-2014_06 |
|---|