| 查看: 826 | 回复: 8 | |||
| 当前主题已经存档。 | |||
| 【悬赏金币】回答本帖问题，作者kelly2243将赠送您 11 个金币 | |||
| 当前只显示满足指定条件的回帖，点击这里查看本话题的所有回帖 | |||
kelly2243木虫 (正式写手)
|
[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）
|
||
|
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 ] |
回复此楼» 猜你喜欢
化工专硕348，一志愿985求调剂
已经有8人回复
-
0856求调剂285
已经有8人回复
-
290求调剂
已经有11人回复
-
281求调剂
已经有7人回复
-
0856化工专硕求调剂
已经有10人回复
-
材料类求调剂
已经有10人回复
-
高分子化学与物理调剂
已经有10人回复
-
321求调剂一志愿东北林业大学材料与化工英二数二
已经有7人回复
-
0856材料求调剂
已经有4人回复
-
化工专硕342，一志愿大连理工大学，求调剂
已经有4人回复
★ ★ ★
kelly2243(金币+3,VIP+0):谢谢.~
kelly2243(金币+3,VIP+0):谢谢.~
|
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
gloria288
木虫 (小有名气)
- 应助: 0 (幼儿园)
- 贵宾: 0.007
- 金币: 2136.7
- 帖子: 194
- 在线: 14.4小时
- 虫号: 500091
- 注册: 2008-02-13
- 专业: 天然有机化学
2楼2008-08-09 15:57:26
★
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
|
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
金虫 (著名写手)
- 应助: 0 (幼儿园)
- 金币: 1034.4
- 帖子: 1247
- 在线: 1.4小时
- 虫号: 405848
- 注册: 2007-06-18
- 性别: MM
- 专业: 外国语言
★ ★ ★ ★ ★ ★ ★ ★ ★ ★
kelly2243(金币+10,VIP+0):ytyt谢谢，有劳啦。
kelly2243(金币+10,VIP+0):ytyt谢谢，有劳啦。
|
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
