±±¾©Ê¯ÓÍ»¯¹¤Ñ§Ôº2026ÄêÑо¿ÉúÕÐÉú½ÓÊÕµ÷¼Á¹«¸æ
²é¿´: 852  |  »Ø¸´: 8
µ±Ç°Ö÷ÌâÒѾ­´æµµ¡£
¡¾ÐüÉͽð±Ò¡¿»Ø´ð±¾ÌûÎÊÌ⣬×÷Õßkelly2243½«ÔùËÍÄú 11 ¸ö½ð±Ò
µ±Ç°Ö»ÏÔʾÂú×ãÖ¸¶¨Ìõ¼þµÄ»ØÌû£¬µã»÷ÕâÀï²é¿´±¾»°ÌâµÄËùÓлØÌû

kelly2243

ľ³æ (ÕýʽдÊÖ)

[ÇóÖú] ±»±à¼­¾Ü¸å˵·­Òë²»µØµÀ£¨»¯Ñ§·½Ã棬ʵÑ鲿·Ö,ÏÖÔÚÒѾ­²î²»¶à·­ÍêÁË,лл£©

¢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 ]

» ²ÂÄãϲ»¶

ÒÑÔÄ   »Ø¸´´ËÂ¥   ¹Ø×¢TA ¸øTA·¢ÏûÏ¢ ËÍTAºì»¨ TAµÄ»ØÌû

furongchun

½ð³æ (ÖøÃûдÊÖ)

лл½ð±Ò£¬²»¹ýÎÒÈÏΪ£¬joinÒ»°ãÔÚ»¯¹¤·­ÒëÖв»×÷Ϊ¼ÓÈëµÄ×îºÃ·­Òë
¡°Ã¿Ò»ÖÖ¾­Ñ飬¶¼ÊÇÒ»Öֳɾ͡£¡±²¥ÏÂÒ»ÖÖ˼Ï룬ÊÕ»ñÒ»ÖÖÐÐΪ¡£²¥ÏÂÒ»ÖÖÐÐΪ¡£ÊÕ»ñÒ»ÖÖϰ¹ß¡£²¥ÏÂÒ»ÖÖϰ¹ß£¬ÊÕ»ñÒ»ÖÖÐÔ¸ñ¡£²¥ÏÂÒ»ÖÖÐÔ¸ñ£¬ÊÕ»ñÒ»ÖÖÃüÔË¡£
7Â¥2008-08-17 14:56:39
ÒÑÔÄ   »Ø¸´´ËÂ¥   ¹Ø×¢TA ¸øTA·¢ÏûÏ¢ ËÍTAºì»¨ TAµÄ»ØÌû
²é¿´È«²¿ 9 ¸ö»Ø´ð

gloria288

ľ³æ (СÓÐÃûÆø)

¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï
kelly2243(½ð±Ò+8,VIP+0):лл£¬È·ÊµºÃ¿´µã£¬Ð»Ð»
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
ÒÑÔÄ   »Ø¸´´ËÂ¥   ¹Ø×¢TA ¸øTA·¢ÏûÏ¢ ËÍTAºì»¨ TAµÄ»ØÌû

demonlcy

ľ³æ (СÓÐÃûÆø)

¡ï
kelly2243(½ð±Ò+1,VIP+0):·þÁËÄ㣬Ä㶼û¸Ä£¬·´ÕýÎÒû·¢Ïָġ£¼ÓÒ»¸öллÄãµÄ¹Ø×¢
¢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 ]
³¤¿ÕÑ©ÂÒÆ®
3Â¥2008-08-12 05:52:16
ÒÑÔÄ   »Ø¸´´ËÂ¥   ¹Ø×¢TA ¸øTA·¢ÏûÏ¢ ËÍTAºì»¨ TAµÄ»ØÌû

furongchun

½ð³æ (ÖøÃûдÊÖ)

¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï
kelly2243(½ð±Ò+10,VIP+0):ytytлл£¬ÓÐÀÍÀ²¡£
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)¡£

¡¡¡¡
¡°Ã¿Ò»ÖÖ¾­Ñ飬¶¼ÊÇÒ»Öֳɾ͡£¡±²¥ÏÂÒ»ÖÖ˼Ï룬ÊÕ»ñÒ»ÖÖÐÐΪ¡£²¥ÏÂÒ»ÖÖÐÐΪ¡£ÊÕ»ñÒ»ÖÖϰ¹ß¡£²¥ÏÂÒ»ÖÖϰ¹ß£¬ÊÕ»ñÒ»ÖÖÐÔ¸ñ¡£²¥ÏÂÒ»ÖÖÐÔ¸ñ£¬ÊÕ»ñÒ»ÖÖÃüÔË¡£
4Â¥2008-08-12 10:34:02
ÒÑÔÄ   »Ø¸´´ËÂ¥   ¹Ø×¢TA ¸øTA·¢ÏûÏ¢ ËÍTAºì»¨ TAµÄ»ØÌû
²»Ó¦Öú È·¶¨»ØÌûÓ¦Öú (×¢Ò⣺ӦÖú²Å¿ÉÄܱ»½±Àø£¬µ«²»ÔÊÐí¹àË®£¬±ØÐëÌîд15¸ö×Ö·ûÒÔÉÏ)
×î¾ßÈËÆøÈÈÌûÍÆ¼ö [²é¿´È«²¿] ×÷Õß »Ø/¿´ ×îºó·¢±í
[¿¼ÑÐ] 304Çóµ÷¼Á +7 ËØÄê¼ÀÓï 2026-04-06 10/500 2026-04-06 23:31 by ËØÄê¼ÀÓï
[¿¼ÑÐ] 286Çóµ÷¼Á +13 Faune 2026-04-06 13/650 2026-04-06 22:35 by chenzhimin
[¿¼ÑÐ] 085405Èí¼þ¹¤³Ì301·ÖÇóµ÷¼Á£¬×¨Ë¶¿É¿çרҵ£¬ËÄÁù¼¶Òѹý +3 ¾²¾²ÏëÏë 2026-04-05 3/150 2026-04-06 15:23 by nepu_uu
[¿¼ÑÐ] Çóµ÷¼Á +5 wos666 2026-04-03 5/250 2026-04-06 10:13 by À¶ÔÆË¼Óê
[¿¼ÑÐ] ²ÄÁϵ÷¼Á +6 Ò»ÑùYWY 2026-04-05 6/300 2026-04-05 20:30 by ÄϺ½~ÍòÀÏʦ
[¿¼ÑÐ] 298Çóµ÷¼Á +7 manman511 2026-04-05 7/350 2026-04-05 10:29 by ÌÆãå¶ù
[¿¼ÑÐ] ÉúÎ﹤³ÌÇóµ÷¼Á +6 ϲ»¶»¹ÊDz»¸ÊÐÄ 2026-04-05 6/300 2026-04-05 10:28 by ÌÆãå¶ù
[¿¼ÑÐ] µ÷¼Á +8 ÐܶþÏëÉϰ¶ 2026-04-04 8/400 2026-04-05 05:27 by houyaoxu
[¿¼ÑÐ] 344²ÄÁÏÓ뻯¹¤µ÷¼Á +9 µ÷¼ÁÉϰ¶«^ 2026-04-03 9/450 2026-04-04 23:10 by happyddm
[¿¼ÑÐ] 296²ÄÁÏר˶Çóµ÷¼Á +21 202451007219 2026-04-02 22/1100 2026-04-04 21:48 by hemengdong
[¿¼ÑÐ] 319Çóµ÷¼Á +4 ÐÇÐDz»Õ£ÑÛà¶ 2026-04-03 4/200 2026-04-04 16:25 by ÖзÉÔº¿Õ¹ÜѧԺÑ
[¿¼ÑÐ] ÍÁľ304Çóµ÷¼Á +4 ÍÃͻͻͻ£¬ 2026-03-31 4/200 2026-04-04 13:34 by 1753564080
[¿¼ÑÐ] 305Çóµ÷¼Á +3 77Qi 2026-04-03 3/150 2026-04-03 23:01 by qzxyhcsy
[¿¼ÑÐ] 357Çóµ÷¼Á +13 1050389037 2026-04-03 13/650 2026-04-03 22:27 by Î޼ʵIJÝÔ­
[¿¼ÑÐ] 293Çóµ÷¼Á +5 ĩδmm 2026-04-02 6/300 2026-04-03 15:20 by Íõ±£½Ü33
[¿¼ÑÐ] 366Çóµ÷¼Á +7 sbdnd 2026-04-03 7/350 2026-04-03 12:40 by cymywx
[¿¼ÑÐ] 274Çóµ÷¼Á +10 Ѧ¶¨Ú̵Ļ¢¡£ 2026-04-01 10/500 2026-04-03 10:13 by tianyyysss
[¿¼ÑÐ] Çóµ÷¼Á0703 +5 ÖܼÎÒ¢ 2026-03-31 8/400 2026-04-01 20:32 by ltltkkk
[¿¼ÑÐ] Ò»Ö¾Ô¸Î÷½»´ó080500²ÄÁÏѧ˶349 +6 jqx1258 2026-03-31 7/350 2026-03-31 21:08 by yuq
[¿¼ÑÐ] 269Çóµ÷¼Á +4 ÎÒÏë¶ÁÑÐ11 2026-03-31 4/200 2026-03-31 10:04 by cal0306
ÐÅÏ¢Ìáʾ
ÇëÌî´¦ÀíÒâ¼û