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kelly2243木虫 (正式写手)
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[求助]
被编辑拒稿说翻译不地道（化学方面，实验部分,现在已经差不多翻完了,谢谢）
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Ⅰ Equipped with a magnetic stirrer in 50 ml flask, Join compounds (1a~b or 1c~d) and using dried DMF dissolved. This mixture cooled to 0℃，then adding 1.1 mol NaH，After the hydrogen volatiled ,stirred at room temperature for 1 h. Ⅱ Added 1.2-2 mol B to the above mixture，room temperature for 18-29 hours stirring (monitored by TLC).Add water to stop the reaction，third extraction with ethyl acetate ; organic layer dried with MgSO4 ,purified by column chromatography，ether recrystallization. Ⅰ 在装有磁力搅拌器的50ml烧瓶中,加入化合物(1a~b或1c~d)并用干燥的DMF溶解,此混合液冷却至0℃后，小心加入两倍物质的量的NaH，待氢气挥发完毕后，在室温条件下搅拌1h。 Ⅱ 再往上述混合液中加入等物质的量的B，室温条件下搅拌22小时(TLC跟踪)。加水使反应停止，用乙酸乙酯萃取三次；有机层用无水MgSO4干燥，溶液旋蒸后柱层析，乙醚重结晶。 Under N2,the reaction was carried out three-neck round-bottom flash (250mL) equipped with thermometer 、condenser tube ,then join compounds(2a~b or 2c~d) dissolving dried 20mL of CH3CN ,2mol Et3N、10mol% Pd(OAc)2，30mol%PPh3, the stirring was continued for 6 hours (monitored by TLC )at 85±0.5 ℃.The mixture was filter and concentrated ,the product was purified by column chromatography. 在装有磁力搅拌器、回流冷凝管和温度计的50ml的三颈烧瓶中,加入化合物(2a~b或2c~d)和两倍物质的量的Et3N、10mol%的Pd(OAc)2，30mol%pph3,并用干燥的甲苯溶解，混合液在氮气氛中、85℃条件下加热回流搅拌6h。反应毕，将混合液经过滤、溶剂旋蒸后得到粗产物，再经过柱层析提纯得到目标化合物(3ab或3c~d)。 South African Journal of Chemistry http://journals.sabinet.co.za/sajchem/chem_aut.html要投的期刊～谢谢。 [ Last edited by kelly2243 on 2008-8-23 at 08:06 ] |
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gloria288
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2楼2008-08-09 15:57:26
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kelly2243(金币+1,VIP+0):服了你，你都没改，反正我没发现改。加一个谢谢你的关注
kelly2243(金币+1,VIP+0):服了你，你都没改，反正我没发现改。加一个谢谢你的关注
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Ⅰ Join compounds (1a~b or 1c~d) to 50 ml flask equipped with magnetic stirrer and using dried DMF for dissolving. After the mixture cooled to 0℃，adding 1.1 mol NaH， when the hydrogen volatiled ,stirred for 1 h at room temperature. Ⅱ Added 1.2-2 mol B to the above mixture， stirring at room temperature for 18-29 hours (monitored by TLC).Add water to stop the reaction， extracting three times with ethyl acetate ; dry the organic layer with dried MgSO4 ,then purified by column chromatography，and ether recrystallization. Under N2,the reaction was carried out in three-neck round-bottom flash (250mL) equipped with thermometer and condenser tube , join compounds(2a~b or 2c~d) dissolving dried 20mL of CH3CN ,2mol Et3N、10mol% Pd(OAc)2，30mol%PPh3, the stirring was continued for 6 hours (monitored by TLC )at 85±0.5 ℃.The mixture was filtered and concentrated ,then the product was purified by column chromatography. 困那...术语我没有查了，感觉前面两段怎么像是机器翻译的？ [ Last edited by demonlcy on 2008-8-12 at 05:53 ] |
3楼2008-08-12 05:52:16
furongchun
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kelly2243(金币+10,VIP+0):ytyt谢谢，有劳啦。
kelly2243(金币+10,VIP+0):ytyt谢谢，有劳啦。
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我的译本： Ⅰ Put compounds (1a~b or 1c~d) into 50 ml flask equipped with a magnetic stirrer, and dissolved with dry DMF. after cooling the mixture to 0℃， added twice mols of NaH，After the hydrogen volatilization,stirred at room temperature for 1 h. Ⅰ 在装有磁力搅拌器的50ml烧瓶中,加入化合物(1a~b或1c~d)并用干燥的DMF溶解,此混合液冷却至0℃后，小心加入两倍物质的量的NaH，待氢气挥发完毕后，在室温条件下搅拌1h。 Ⅱ Added same mol of B to the above mixture，stirred under room temperature for 18-29 hours (monitored by TLC).Added water to stop the reaction， extracted with ethyl acetate for three times; dried the organic layer with Anhydrous Magnesium, after concentration, purified by column chromatography，and recrystallized with ether Ⅱ 再往上述混合液中加入等物质的量的B，室温条件下搅拌22小时(TLC跟踪)。加水使反应停止，用乙酸乙酯萃取三次；有机层用无水MgSO4干燥，溶液旋蒸后柱层析，乙醚重结晶。 Under N2,the reaction was carried out in three-neck round-bottom flask (250mL) equipped with thermometer 、condenser tube ,then added compounds(2a~b or 2c~d) ,dissolving with dry 20mL of CH3CN ,2mol Et3N、10mol% Pd(OAc)2，30mol%PPh3, the stirring was continued for 6 hours (monitored by TLC )at 85±0.5 ℃.The mixture was filtered and concentrated ,the product was purified by column chromatography. 在装有磁力搅拌器、回流冷凝管和温度计的50ml的三颈烧瓶中,加入化合物(2a~b或2c~d)和两倍物质的量的Et3N、10mol%的Pd(OAc)2，30mol%pph3,并用干燥的甲苯溶解，混合液在氮气氛中、85℃条件下加热回流搅拌6h。反应毕，将混合液经过滤、溶剂旋蒸后得到粗产物，再经过柱层析提纯得到目标化合物(3ab或3c~d)。 |
4楼2008-08-12 10:34:02
chengcj.2008
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kelly2243(金币+15,VIP+0):谢谢，有劳啦
kelly2243(金币+15,VIP+0):谢谢，有劳啦
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仅作参考: Ⅰ Compounds (1a~b or 1c~d) in dry DMF were added to a 50 mL flask equipped with a magnetic stirrer. The above mixture were cooled to 0℃，followed by adding 2.0 equivalent NaH (1.1 mol). After no hydrogen bubble was formed, the resulting mixture was stirred at room temperature for 1 h. Ⅱ To the above mixture, equal molar B (1.2-2 mol ), and the reaction system was stirred at room temperature for 18-29 hours (monitored by TLC). Then, the reaction was quenched by adding water, extracted three times with ethyl acetate. The organic layer was dried over anhydrous MgSO4, evapourated in vacuo, and the residue was purified by column chromatography, recrystallized in ether. To a three-necked round-bottom flask (250mL or 50 mL) equipped with thermometer and condenser were added compounds (2a~b or 2c~d) dissolved in dry CH3CN (20mL), Et3N (2mol)、 Pd(OAc)2 (10mol%)， PPh3 (30mol%), and dry toluene, respectively. The mixture was stirred at 85±0.5 ℃ for 6h under N2 atmosphere (monitored by TLC ). Then, the reaction mixture was filtered and concentrated , and the crude product was purified on column chromatography. |
5楼2008-08-12 10:42:39
6楼2008-08-17 09:41:50
furongchun
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7楼2008-08-17 14:56:39
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kelly2243(金币+3,VIP+0):谢谢.~
kelly2243(金币+3,VIP+0):谢谢.~
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ⅠAdd compounds 1a~b or 1c~d into a 50 ml flask equipped with a magnetic stirrer, and allow to dissolve in dry DMF. after allowing to cool the mixture to 0℃， carefully add two equivalent NaH. After hydrogen evaporates completely, stir at room temperature for 1 h. Ⅱ Add equivalent B to the above mixture，stir at room temperature for 22 hours and monitor by TLC regularly. Add water to stop the reaction， extract with ethyl acetate for three times; And then obtain compounds 2a~b or 2c~d after a series of work up procedures, such as dessication of organic layer with Anhydrous Magnesium, concentration, purification by column chromatography and re-crystallization in ether. Add compounds 2a~b or 2c~d , two equivalent Et3N, 10% (mol)of Pd(OAc)2 and 30% (mol) PPh3 into a 50 ml flask equipped with a magnetic stirrer, condenser and thermometer, and allow to dissolve in dry toluene. Allow the mixture to reflux for 6h at 85℃ in the presence of nitrogen while stirring. And finally obtain target compound 3a~b or 3c~d after the mixture is subject to filtration, concentration to crude product, and purification by column chromatography. |
8楼2008-08-21 18:33:58
