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Bromine → Ethyl 8-bromo-2,2-dimethylchroman-6-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Ethyl 2,2-dimethylchroman-6-carboxylate | HCID 246672 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Ethyl 8-bromo-2,2-dimethylchroman-6-carboxylate | HCID 10519233 | 110.6% |
反応手順
To a solution of ethyl 2,2-dimethylchroman-6-carboxylate (Compound 216, 500 mg, 2.14 mmol) in HOAc (4 mL) was added Br2 (0.11 mL, 2.14 mmol). The reaction mixture was stirred at room temperature overnight and then a stream of air was passed through the reaction mixture to remove the excess Br2. Removal of the solvent under reduced pressure and column chromatography using the residue (EtOAc:hexanes1:9) afforded 741 mg (100%) of the title compound as an oil. 1H NMR δ 8.05 (1H, d, J=2.2 Hz), 7.73 (1H, d, J=2.2 Hz), 4.34 (2H, q, J=7.1 Hz), 2.84 (2H, t, J=6.7 Hz), 1.85 (2H, t, J=6.7 Hz), 1.40 (6H, s), 1.38 (3H, t, J=7.2 Hz). Anal (C14H17BrO3.0.2 H2O) C, H.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05877207 |
| 出典データセット | uspto-grants-1999_03 |
| ORD ID | ord-86a21189e8e74b7888003b54e41c64e4 |
| 出典メモ | uspto-grants-1999_03 |