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xl2088131新蟲(chóng) (著名寫手)
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[求助]
幫忙翻譯一下如何操作
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Hexamethyldisilazane 1.84 g (0.012 mol) was added to acetic acid (14 ml) and acetylacetone 1.20 g (0.012 mol) at an appropriate rate to maintain the internal temperature at 70 ◦C. The HMDS and acetic acid mixture was added to a solution of acetylacetone 1.20 g (0.012 mol) and malononitrile 3.17 g (0.048 mol) in acetic acid (14 ml). After 3 h, the mixture was cooled to ambient temperature and washed four times with water. And the residue was isolated by crystallization in CH3CN. Yield 85%. |
捐助貴賓 (正式寫手)
木蟲(chóng) (小有名氣)
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向14mL 乙酸和1.20 g(0.012 mol)乙酰丙酮的混合物中緩慢加入1.84 g(0.012 mol)六甲基二硅氮烷,添加過(guò)程中要保持混合物的溫度在70℃.將上述混合物加入到1.20 g(0.012 mol)乙酰丙酮和3.17 g (0.048 mol)丙二腈的乙酸(14 mL)溶液中。3個(gè)小時(shí)后,把新混合物冷卻至室溫,用水洗滌四次后,將剩余固體在乙腈中溶解,重新結(jié)晶以分離雜質(zhì)。重結(jié)晶過(guò)程回收率是85%。 這個(gè)工藝有很多不明白的地方:一是加完六甲基二硅氮烷后,70℃要反應(yīng)多久。二是70℃的原混合物加入到1.20 g(0.012 mol)乙酰丙酮和3.17 g (0.048 mol)丙二腈的乙酸(14 mL)溶液中。加入前,新混合物的溫度是多少,加入后溫度又是多少。加完了,繼續(xù)反應(yīng)3小時(shí)后,是直接加水洗,還是固液分離后,用水洗固體。這些疑問(wèn)都需要慢慢做試驗(yàn)證明。 |
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