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1-(Chloromethoxy)-2-methoxyethane → 3,5-Bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(Chloromethoxy)-2-methoxyethane | HCID 77590 | — |
| 反応物 | Benzonitrile, 3,5-bis(1,1-dimethylethyl)-4-hydroxy- | HCID 137274 | — |
| 反応物 | N,N-Diisopropylmethylamine | HCID 547370 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3,5-Bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile | HCID 10041643 | 97% |
反応手順
2-Methoxyethoxymethyl chloride (4.1 g, 0.032 mole) is added dropwise to a 0° C. mixture of 3,5-bis(1,1-dimethylethyl)-4-hydroxybenzonitrile (Louis A. Cohen, Journal of Organic Chemistry 22, 1333, 1957) (5.0 g, 0.022 mole) and diisopropylaminomethane (4.2 g, 0.032 mole) in methylene chloride (50 ml). The mixture is allowed to warm to room temperature and stir 18 hours. The solution is diluted with methylene chloride (25 ml) and washed with water (25 ml), cold 2M HCl (20 ml), saturated aqueous NaCl, and dried over MgSO4. Filtered and concentrated in vacuo to obtain 6.7 g (6.9 g theor., 97%) of 3,5-bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05155122 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-edcad62bf0124dd18582110a8b7b330a |
| 出典メモ | uspto-grants-1992_10 |