関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Anisole | HCID 7519 | — |
| 反応物 | 4-Bromobenzoyl chloride | HCID 68515 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Bromo-4'-methoxybenzophenone | HCID 794333 | — |
反応手順
To a cooled (0° C.) mixture of 4-bromobenzoyl chloride, 1-1-a, (25 g, 0.114 mol) and anisole (15.5 g, 0.143 mol) in DCM (500 ml) was added AlCl3 (19 g, 0.143 mol) portion wise with stirring under N2. The resulting reaction mixture was allowed to stir at r.t for 16 h. The reaction mixture was poured into 20% HCl (500 ml) and the solution stirred for 1 h. After stirring, the resulting solution was allowed to separate into phase layers. The aqueous layer was collected and further extracted with DCM (3×250 ml). The combined organic layer was washed with water (200 ml), brine (200 ml), dried (Na2SO24), filtered and concentrated under reduced pressure to yield 30 g of a white solid, 1-1-b. 1H NMR (300 MHZ, CDCl3): 3.91 (s, 3H), 6.99 (d, 2H), 7.65 (s, 4H), 7.82 (d, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09079930B2 |
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| 出典データセット | uspto-grants-2015_07 |
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| ORD ID | ord-6fe08ff10f8f43e795b8810648a77ae1 |
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| 出典メモ | uspto-grants-2015_07 |
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