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Hydrochloric Acid → 1-[3-Tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-tert-butyl-N-methoxy-5-(2-methoxyethoxy)-N-methylbenzamide | HCID 58136801 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-[3-Tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone | HCID 58136808 | — |
反応手順
3-tert-Butyl-N-methoxy-5-(2-methoxyethoxy)-N-methylbenzamide (O3.043; 1.35 g) was dissolved in THF (40 ml), methylmagnesium bromide (3.05 ml, 3 M in ether) was added dropwise at 0° C. and then the mixture was stirred at RT for 2 h. Then the mixture was admixed with 1 N hydrochloric acid (50 ml), diluted with water and extracted by shaking three times with EA. Then the combined EA phases were dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (40 g cartridge, n-heptane/EA gradient of 0-30% in 30 min). 1.0 g of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08076336B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-82c79826129b4f49a7366ce680b36a0a |
| 出典メモ | uspto-grants-2011_12 |