最近在做CDI(羰基二咪唑)，活化4-羥甲基頻哪醇酯，得到活化酯，一開(kāi)始按文獻(xiàn)是可以制備得到固體產(chǎn)物的，可最近可能氣溫降低還是原材料變質(zhì)，按原方法，萃取，無(wú)水硫酸鈉吸水后，旋干乙酸乙酯后，始終無(wú)法得到固體，僅有一些液體狀粘稠物，像凝膠，嘗試延長(zhǎng)反應(yīng)時(shí)間，提高CDI比例仍無(wú)改善，不知有沒(méi)有朋友做過(guò)類(lèi)似反應(yīng)，求教，十分感謝。
以下為文獻(xiàn)方法：Compound S1 (7.37 g, 31.5 mmol) was dissolved in dry CH2Cl2 (46 mL) in a flame-dried 100-mL flask. Carbonyldiimidazole (10.20 g, 62.9 mmol) was added and the reaction was stirred for 30 min. The mixture was diluted in ethyl acetate (200 mL) and washed with H2O (3 x 10 mL). The organics were washed with brine (1 x 10 mL), dried over MgSO4, and concentrated in vacuo to give a pure white solid@celan@celan@celan@celan@yangtie2008 返回小木蟲(chóng)查看更多