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Methyl formate → (Z)-methyl 2-(hydroxymethylene)butanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl formate | HCID 7865 | — |
| 反応物 | Methyl butyrate | HCID 12180 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | (Z)-methyl 2-(hydroxymethylene)butanoate | HCID 22056702 | 46.2% |
反応手順
To a suspension of NaH (7.99 g, 200 mmol) in DME (100 mL) was added a mixture of methyl butyrate (5.1 g, 49.9 mmol) and methyl formate (17.99 g, 300 mmol) in DME (100 mL) dropwise at 0° C. under nitrogen. The mixture was stirred at room temperature overnight, and then filtered through a pad of celite. To the filtrate was added ether (200 mL), and let the suspension stand for 4 h. The solid was collected by filtration, washed with diethyl ether and dried in vacuo to afford the title compound (3 g, 23.05 mmol). LCMS: rt=1.108 min, [M+H+]=130
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08637536B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-2c088e74e59c4baea156540dfdf371c7 |
| 出典メモ | uspto-grants-2014_01 |