32454-36-7
32454-36-7 結(jié)構(gòu)式
基本信息
ethyl 2-(4-broMophenyl)-2-Methylpropanoate
Benzeneacetic acid, 4-bromo-α,α-dimethyl-, ethyl ester
制備方法
14062-25-0
74-88-4
32454-36-7
實(shí)施例13A 2-(4-溴苯基)-2-甲基丙酸乙酯的合成:將2.0 g (8.2 mmol) 對(duì)溴苯乙酸乙酯溶解于50 mL DMF中,在室溫下緩慢加入0.7 g (18 mmol) 60%氫化鈉礦物油懸浮液。混合物在室溫下攪拌30分鐘后,加入2.9 g (20.6 mmol) 碘甲烷。反應(yīng)混合物在室溫下繼續(xù)攪拌過(guò)夜。反應(yīng)完成后,用乙酸乙酯稀釋反應(yīng)混合物,依次用水和飽和氯化鈉溶液萃取。分離有機(jī)相,用無(wú)水硫酸鎂干燥,過(guò)濾后濃縮濾液。殘余物通過(guò)制備型HPLC [Reprosil C18, 10 μm, 250 mm × 40 mm, 梯度洗脫(30%甲醇/70%水至100%甲醇), 運(yùn)行時(shí)間25分鐘]進(jìn)行純化。經(jīng)HPLC分析后,合并含有目標(biāo)產(chǎn)物的餾分并濃縮,得到1.75 g (產(chǎn)率78%) 油狀產(chǎn)物。產(chǎn)物通過(guò)GC-MS [方法5] 和1H-NMR (400 MHz, DMSO-d6) 進(jìn)行表征:GC-MS: Rt = 5.10分鐘; MS (ESIpos): m/z = 270/272 [M+]; 1H-NMR: δ [ppm] = 1.11 (t, 3H), 1.48 (s, 6H), 4.06 (q, 2H), 7.24-7.29 (m, 2H), 7.50-7.54 (m, 2H)。
參考文獻(xiàn):
[1] Patent: US2016/318866, 2016, A1. Location in patent: Paragraph 0639; 0640; 0641
[2] Patent: WO2011/44187, 2011, A1. Location in patent: Page/Page column 94
[3] Patent: WO2013/40790, 2013, A1. Location in patent: Page/Page column 60
[4] Patent: WO2013/43624, 2013, A1. Location in patent: Page/Page column 59; 60
[5] Patent: EP3239143, 2017, A2. Location in patent: Paragraph 0339
| 報(bào)價(jià)日期 | 產(chǎn)品編號(hào) | 產(chǎn)品名稱(chēng) | CAS號(hào) | 包裝 | 價(jià)格 |
| 2026/06/05 | XW023245436703 | 2-(4-溴苯基)-2-甲基丙酸乙酯 Ethyl 2-(4-bromophenyl)-2-methylpropanoate | 32454-36-7 | 1g | 500元 |
| 2026/06/05 | XW023245436702 | 2-(4-溴苯基)-2-甲基丙酸乙酯 Ethyl 2-(4-bromophenyl)-2-methylpropanoate | 32454-36-7 | 250mg | 125元 |
| 2026/06/05 | XW023245436701 | 2-(4-溴苯基)-2-甲基丙酸乙酯 Ethyl 2-(4-bromophenyl)-2-methylpropanoate | 32454-36-7 | 100mg | 52元 |