関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl 7-hydroxy-2-oxo-2H-1-benzopyran-3-carboxylate | HCID 5416969 | — |
| 生成物 | HCID 9972651 | HCID 9972651 | 135.4% |
反応手順
7-hydroxyl-3-coumarin carboxylic acid methyl ester (0.2g, 1 mmol) is dissolved in N,N′-dimethyl formamide (2 mL), and bromobenzyl (0.36 ml, 3 mmol) and levigated potassium carbonate (0.5 g) are added into. The resulting mixture is stirred for 12 hours at 70° C. After adding 10 mL of water, extraction is conducted with ethyl acetate, and all of ethyl acetate are combined, followed by washing with water, drying on anhydrous sodium sulfate. Then the solution is concentrated under reduced pressure to approximately 5 mL and is placed to separate out a solid, followed by filtering under reduced pressure to obtain 0.21 g of the captioned compound, yield: 67.7%. m.p.129-130° C. 1H NMR(CDCl3): δ=3.92(s, 3H), 5.19(s, 2H), 6.85(d, J=2.4 Hz, 1H), 6.95(dd, J=8.8 Hz, 2.4 Hz, 1H), 7.40(m, 5H), 7.52(d, J=8.8 Hz, 1H), 8.55(s, 1H); Elements Analysis, C18H14O5 (310): Calculated C, 69.68; H, 4.52. Found C, 69.63; H, 4.51; IR(KBr) : 3054.7, 2948.7, 1749.1, 1697.1, 1610.3, 1558.2, 1500.4, 1438.7, 1378.9, 1226.5, 1116.6, 1026, 794.5, 725.1, 692.3, 636.4 cm−1; EI-MS(m/z): 310(12, M+), 91(100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07456205B2 |
|---|
| 出典データセット | uspto-grants-2008_11 |
|---|
| ORD ID | ord-b5868d1c83b64a8491d1c9c3acfaf368 |
|---|
| 出典メモ | uspto-grants-2008_11 |
|---|