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Ammonia → (3-((Tert-butyldimethylsilyloxy)methyl)phenyl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | 1,3-Benzenedimethanol | HCID 69374 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (3-((Tert-butyldimethylsilyloxy)methyl)phenyl)methanol | HCID 10658493 | 45.4% |
反応手順
To 1,3-benzenedimethanol (5.10 g, 36.91 mmol) in dichloromethane (70 ml) was added at 0° C. triethylamine (7.47 g, 73.82 mmol), 4-dimethyl-aminopyridine (451 mg, 3.61 mmol) and t-butyldimethylchlorosilane (5.56 g, 36.91 mmol) successively, and the mixture was stirred for 20 hours at room temperature. Thereto was added a saturated ammonia solution and the mixture was extracted with ethyl acetate and separated by a separating funnel. The organic layer was washed with water and saturated brine, dried over magnesium sulfate and filtered. The solvent was removed in vacuo and the residue was purified by silica gel column chromatography to give the subject compound (4.23 g, 45%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07781479B2 |
| 出典データセット | uspto-grants-2010_08 |
| ORD ID | ord-50fc8bbb3b3b47048f33b51ad57a2c25 |
| 出典メモ | uspto-grants-2010_08 |