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Ethyl orthoformate → HCID 15114404、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl orthoformate | HCID 31214 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 2-Bromo-5-(trifluoromethyl)benzaldehyde | HCID 7018047 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 15114404 | HCID 15114404 | 71% |
反応手順
Step AJ (1): 2-Bromo-5-(trifluoromethyl)benzaldehyde (1069 mg, 4.975 mmol) was dissolved in a mixture of methanol (20 mL) and triethylorthoformate (20 mL). p-Toluenesulfonic acid monohydrate (180.0 mg, 0.946 mmol) was added and the reaction mixture was stirred under reflux for 5 h. The reaction was quenched with aqueous NaHCO3 and extracted with DCM. The combined organic phases were dried over Na2SO4, filtered and concentrated in vacuum at the temperature, not exceeding 35° C. The residue was purified by silica gel chromatography to give 1-bromo-2-(dimethoxymethyl)-4-methoxybenzene (1060 mg, 71%) as a colorless oil. LC-MS (M−OCH3)+=267.23.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07772221B2 |
| 出典データセット | uspto-grants-2010_08 |
| ORD ID | ord-25ca6c9a1559491c99e95eb8418e6fef |
| 出典メモ | uspto-grants-2010_08 |