関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzoic acid, 3,5-dihydroxy-, ethyl ester | HCID 20098 | — |
| 反応物 | 4-(Bromomethyl)benzonitrile | HCID 86996 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3,5-Bis(4-cyanophenoxy)benzoic acid ethyl ester | HCID 66818480 | 83% |
反応手順
To a solution of 3,5-dihydroxy benzoic acid ethyl ester 1.2 g (6.58 mmol), dissolved in 10 ml DMF, was added K2CO3 3.63 g (26.32 mmol) followed by 4-bromomethyl-benzonitrile 5.16 g (26.32 mmol) in 5 ml of DMF at 20° C. The reaction mixture was allowed to attain RT and then heated to 35° C. for 8 h. The solvent was removed under reduced pressure and the residue was dissolved in 200 ml of ethyl acetate. The organic layer was washed with brine and water. Organic phase was dried over anhydrous sodium sulphate and solvent was removed under reduced pressure. The crude product was subjected to column chromatography and eluted using hexane:ethyl acetate (8:2) to afford 2.1 g of purified product. 1H NMR (DMSO-d6): 1.3 (3H, t), 4.3 (2H, q), 5.3 (4H, s), 7.0 (1H, s), 7.18 (2H, s), 7.64 (4H, d), 7.86 (4H, d).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08722930B2 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-b5c6d602a92b44d98da914997540678f |
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| 出典メモ | uspto-grants-2014_05 |
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