| 查看: 408 | 回复: 3 | |||
| 当前主题已经存档。 | |||
bad2266金虫 (正式写手)
~残菊~
|
[交流]
摘要 ！急！！！5月30号15点之前
|
||
|
以杉木根为原料通过水蒸气蒸馏法提取杉木精油，从杉木根精油中精制提取柏木脑，再以柏木脑为原料合成甲基柏木醚。 对于杉木根精油的提取，目前国内外文献报道几乎都是用水蒸气法提取，精油提取率仅为1.9~2.1%。本实验尝试使用尿素水溶液浸泡杉木根后再用水蒸气法提取杉木根精油。用50%的尿素浸泡杉木根一小时后对其进行精油提取，精油提取率可达5.4%。 本文采用氨基钠法合成甲基柏木醚。反应分两步，首先氨基钠与柏木脑反应生成醇钠，然后醇钠与硫酸二甲酯进行甲基化反应生成甲基柏木醚。通过多组单因素实验发现氨基钠：柏木脑：硫酸二甲酯的摩尔比为1.6：1：0.9，第一步反应条件控制在回流2h，第二步反应先室温（25℃）滴加硫酸二甲酯后反应1h，再回流反应1h，得率可达88.8%。本实验对甲基柏木醚氨基钠法工业化生产具有一定的参考价值。 |
回复此楼
|
以杉木根为原料通过水蒸气蒸馏法提取杉木精油，从杉木根精油中精制提取柏木脑，再以柏木脑为原料合成甲基柏木醚。 对于杉木根精油的提取，目前国内外文献报道几乎都是用水蒸气法提取，精油提取率仅为1.9~2.1%。本实验尝试使用尿素水溶液浸泡杉木根后再用水蒸气法提取杉木根精油。用50%的尿素浸泡杉木根一小时后对其进行精油提取，精油提取率可达5.4%。 The fir essential oil was extracted from fir root by steam distillation method, from which cedrol was extracted, and then, cedrol methyl ether was synthesized based on cedrol. The methods for fir essential oil extracting reported in the literatures at home and abroad almost totally referred to steam distillation method and extraction rate for essential oil reached to only 1.9-2.1%. In our experiment, essential oil was attempted to extract from fir immersed in urea solution. Essential oil was extracted from fir root immersed in 50% concentration of urea solution for 1h and essential oil reached to 5.4%. |
2楼2009-05-30 12:52:31
|
本文采用氨基钠法合成甲基柏木醚。反应分两步，首先氨基钠与柏木脑反应生成醇钠，然后醇钠与硫酸二甲酯进行甲基化反应生成甲基柏木醚。通过多组单因素实验发现氨基钠：柏木脑：硫酸二甲酯的摩尔比为1.6：1：0.9，第一步反应条件控制在回流2h，第二步反应先室温（25℃）滴加硫酸二甲酯后反应1h，再回流反应1h，得率可达88.8%。本实验对甲基柏木醚氨基钠法工业化生产具有一定的参考价值。 In this paper, the cedrol methyl ether was synthesized by sodamide method. Two steps were included in this reaction, first, sodium alkoxide was synthesized by th reaction between sodamide and cedrol, then cedrol methyl ether was synthesized by methylation reaction between sodium alkoxide and dimethyl sulfate. Based on groups of single factor experiments, the yield could reached to 88.8% with the conditions: sodamide: cedrol :dimethyl sulfate = 1.6:1:0.9, refluxed 2h in first step reaction, and reacted at room temperature 1h after instillation of dimethyl sulfate, followed refluxed 1h in the second steps. A certain reference value was indicated in this experiment for industry synthesis of cedrol methyl ether by sodamide method. |
3楼2009-05-30 13:18:08
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
bad2266(金币+30,VIP+0):thank you very much~! 5-30 22:48
bad2266(金币+30,VIP+0):thank you very much~! 5-30 22:48
|
汇总起来： The fir essential oil was extracted from fir root by steam distillation method, from which cedrol was extracted, and then, cedrol methyl ether was synthesized based on cedrol. The methods for fir essential oil extracting reported in the literatures at home and abroad almost totally referred to steam distillation method and extraction rate for essential oil reached to only 1.9-2.1%. In our experiment, essential oil was attempted to extract from fir immersed in urea solution. Essential oil was extracted from fir root immersed in 50% concentration of urea solution for 1h and essential oil reached to 5.4%. In this paper, the cedrol methyl ether was synthesized by sodamide method. Two steps were included in this reaction, first, sodium alkoxide was synthesized by th reaction between sodamide and cedrol, then cedrol methyl ether was synthesized by methylation reaction between sodium alkoxide and dimethyl sulfate. Based on groups of single factor experiments, the yield could reached to 88.8% with the conditions: sodamide: cedrol :dimethyl sulfate = 1.6:1:0.9, refluxed 2h in first step reaction, and reacted at room temperature 1h after instillation of dimethyl sulfate, followed refluxed 1h in the second steps. A certain reference value was indicated in this experiment for industry synthesis of cedrol methyl ether by sodamide method. 仅供参考 |
4楼2009-05-30 13:21:01
