関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Phenol, 3-(1,1-dimethylethyl)- | HCID 11450 | — |
| 反応物 | N-Methylol-alpha-chloroacetamide | HCID 62466 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | N-(4-tert-butyl-2-hydroxybenzyl)-2-chloroacetamide | HCID 66746309 | 33% |
反応手順
A mixture of 3-tert-butyl phenol (500.0 mg, 3.33 mmol) and 2-chloro-N-(hydroxymethyl)acetamide (411.2 mg, 3.33 mmol) was added in portions to an ice-bath cold solution of acetic acid (3.0 ml) and conc. H2SO4 (0.5 ml). The mixture was stirred at 0-5° C. for 3.0 h. and then it was allowed to warm to r.t. Stirring continued at r.t. for 20 h. The mixture was poured into ice-water, neutralized with solid NaHCO3 and extracted with CH2Cl2. The combined organic extracts were dried (MgSO4), filtered and concentrated. The crude product was purified by flash chromatography; Pet. Ether, EtOAc (9:1→7:3) affording 278 mg (33%) the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08415333B2 |
|---|
| 出典データセット | uspto-grants-2013_04 |
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| ORD ID | ord-a93edd84edd84cba80beaa554d3866ff |
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| 出典メモ | uspto-grants-2013_04 |
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