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¢ñ 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¡æ£¬then adding 1.1 mol NaH£¬After the hydrogen volatiled ,stirred at room temperature for 1 h. ¢ò 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. ¢ñ ÔÚ×°ÓдÅÁ¦½Á°èÆ÷µÄ50mlÉÕÆ¿ÖÐ,¼ÓÈ뻯ºÏÎï(1a~b»ò1c~d)²¢ÓøÉÔïµÄDMFÈܽâ,´Ë»ìºÏÒºÀäÈ´ÖÁ0¡æºó£¬Ð¡ÐļÓÈëÁ½±¶ÎïÖʵÄÁ¿µÄNaH£¬´ýÇâÆø»Ó·¢Íê±Ïºó£¬ÔÚÊÒÎÂÌõ¼þϽÁ°è1h¡£ ¢ò ÔÙÍùÉÏÊö»ìºÏÒºÖмÓÈëµÈÎïÖʵÄÁ¿µÄB£¬ÊÒÎÂÌõ¼þϽÁ°è22Сʱ(TLC¸ú×Ù)¡£¼Óˮʹ·´Ó¦Í£Ö¹£¬ÓÃÒÒËáÒÒõ¥ÝÍÈ¡Èý´Î£»Óлú²ãÓÃÎÞË®MgSO4¸ÉÔÈÜÒºÐýÕôºóÖù²ãÎö£¬ÒÒÃÑÖØ½á¾§¡£ 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¡À0.5 ¡æ.The mixture was filter and concentrated ,the product was purified by column chromatography. ÔÚ×°ÓдÅÁ¦½Á°èÆ÷¡¢»ØÁ÷ÀäÄý¹ÜºÍζȼƵÄ50mlµÄÈý¾±ÉÕÆ¿ÖÐ,¼ÓÈ뻯ºÏÎï(2a~b»ò2c~d)ºÍÁ½±¶ÎïÖʵÄÁ¿µÄEt3N¡¢10mol%µÄPd(OAc)2£¬30mol%pph3,²¢ÓøÉÔïµÄ¼×±½Èܽ⣬»ìºÏÒºÔÚµªÆø·ÕÖС¢85¡æÌõ¼þϼÓÈÈ»ØÁ÷½Á°è6h¡£·´Ó¦±Ï£¬½«»ìºÏÒº¾¹ýÂË¡¢ÈܼÁÐýÕôºóµÃµ½´Ö²úÎÔÙ¾¹ýÖù²ãÎöÌá´¿µÃµ½Ä¿±ê»¯ºÏÎï(3ab»ò3c~d)¡£ ¡¡¡¡South African Journal of Chemistry¡¡http://journals.sabinet.co.za/sajchem/chem_aut.htmlҪͶµÄÆÚ¿¯¡«Ð»Ð»¡£ [ Last edited by kelly2243 on 2008-8-23 at 08:06 ] |
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demonlcy
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6Â¥2008-08-17 09:41:50
gloria288
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- ½ð±Ò: 2136.7
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| Compounds (1a~b or 1c~d) were dissoved by DMF in a 50ml flask with magnetic strrer. When cooled it to 0¡æ£¬add 1.1 mol NaH£¬and the reaction were carried out for 1h after the hydrogen volatiled. |
2Â¥2008-08-09 15:57:26
demonlcy
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- Ó¦Öú: 1 (Ó×¶ùÔ°)
- ½ð±Ò: 3288.8
- Ìû×Ó: 112
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¢ñ 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¡æ£¬adding 1.1 mol NaH£¬ when the hydrogen volatiled ,stirred for 1 h at room temperature. ¢ò 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¡À0.5 ¡æ.The mixture was filtered and concentrated ,then the product was purified by column chromatography. À§ÄÇ...ÊõÓïÎÒûÓвéÁË£¬¸Ð¾õÇ°ÃæÁ½¶ÎÔõôÏñÊÇ»úÆ÷·ÒëµÄ£¿ [ Last edited by demonlcy on 2008-8-12 at 05:53 ] |

3Â¥2008-08-12 05:52:16
furongchun
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- ½ð±Ò: 1034.4
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- ×¢²á: 2007-06-18
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ÎÒµÄÒë±¾£º ¢ñ 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¡æ£¬ added twice mols of NaH£¬After the hydrogen volatilization,stirred at room temperature for 1 h. ¢ñ ÔÚ×°ÓдÅÁ¦½Á°èÆ÷µÄ50mlÉÕÆ¿ÖÐ,¼ÓÈ뻯ºÏÎï(1a~b»ò1c~d)²¢ÓøÉÔïµÄDMFÈܽâ,´Ë»ìºÏÒºÀäÈ´ÖÁ0¡æºó£¬Ð¡ÐļÓÈëÁ½±¶ÎïÖʵÄÁ¿µÄNaH£¬´ýÇâÆø»Ó·¢Íê±Ïºó£¬ÔÚÊÒÎÂÌõ¼þϽÁ°è1h¡£ ¢ò 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 ¢ò ÔÙÍùÉÏÊö»ìºÏÒºÖмÓÈëµÈÎïÖʵÄÁ¿µÄB£¬ÊÒÎÂÌõ¼þϽÁ°è22Сʱ(TLC¸ú×Ù)¡£¼Óˮʹ·´Ó¦Í£Ö¹£¬ÓÃÒÒËáÒÒõ¥ÝÍÈ¡Èý´Î£»Óлú²ãÓÃÎÞË®MgSO4¸ÉÔÈÜÒºÐýÕôºóÖù²ãÎö£¬ÒÒÃÑÖØ½á¾§¡£ 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¡À0.5 ¡æ.The mixture was filtered and concentrated ,the product was purified by column chromatography. ÔÚ×°ÓдÅÁ¦½Á°èÆ÷¡¢»ØÁ÷ÀäÄý¹ÜºÍζȼƵÄ50mlµÄÈý¾±ÉÕÆ¿ÖÐ,¼ÓÈ뻯ºÏÎï(2a~b»ò2c~d)ºÍÁ½±¶ÎïÖʵÄÁ¿µÄEt3N¡¢10mol%µÄPd(OAc)2£¬30mol%pph3,²¢ÓøÉÔïµÄ¼×±½Èܽ⣬»ìºÏÒºÔÚµªÆø·ÕÖС¢85¡æÌõ¼þϼÓÈÈ»ØÁ÷½Á°è6h¡£·´Ó¦±Ï£¬½«»ìºÏÒº¾¹ýÂË¡¢ÈܼÁÐýÕôºóµÃµ½´Ö²úÎÔÙ¾¹ýÖù²ãÎöÌá´¿µÃµ½Ä¿±ê»¯ºÏÎï(3ab»ò3c~d)¡£ ¡¡¡¡ |

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