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Potassium Carbonate → 3-((4-Bromo-3,5-dimethylphenoxy)methyl)-3-methyloxetane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| 反応物 | Oxetane, 3-(bromomethyl)-3-methyl- | HCID 144860 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-((4-Bromo-3,5-dimethylphenoxy)methyl)-3-methyloxetane | HCID 86697102 | — |
反応手順
To a solution of 4-bromo-3,5-dimethylphenol (3.0 g) and K2CO3 (5.5 g) in N,N-dimethylformamide (10 mL) is added 3-(bromomethyl)-3-methyloxetane (2.95 g). The mixture is stirred for 12 hours at room temperature and then partitioned between saturated aqueous NaHCO3 solution and ethyl acetate. The aqueous phase is extracted with ethyl acetate and the combined organic phases are dried (MgSO4). The solvent is evaporated and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 100:0→70:30) to give the title compound. Yield: 3.5 g; LC (method 4): tR=1.81 min; Mass spectrum (ESI+): m/z=285 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08642585B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-7d867147ffd541b38140cb598cd36b86 |
| 出典メモ | uspto-grants-2014_02 |