ÀÚµ¿·Î±×ÀÎ
ÄÁÅÙÃ÷ | contents
ÀϹݰԽÃÆÇ
Q&A°Ô½ÃÆÇ
°øÇÐ S/W
½ºÅ͵ð | study
´ÜÀ§È¯»ê
³óµµ°è»ê
ÀϹÝÈ­ÇÐ
È­°øÀϹÝ
È­°ø½Ç¹«

   
  Bropentane°ú indoleÀÇ ÇÕ¼º
  ±Û¾´ÀÌ : Á¶Àºº°   °íÀ¯ID : Jebjjang     ³¯Â¥ : 13-01-29 13:24     Á¶È¸ : 4546    

To a stirred solution of 5.00 g (42.7 mmol) of indole in 10 mL of DMSO was added 10.8 g (192 mmol) of crushed KOH. Addition of 12.9 g (85.4 mmol) of 1-bromopentane was followed by stirring at ambient temperature for 1.5 h under N2. The reaction was quenched with water and the product was extracted with 3 portions of dichloromethane. The organic layer was dried (MgSO4) and concentrated in vacuo. Kugelrohr distillation at 200 ¡ÆC under 19 in. Hg gave 8.15 g (98%) of N-pentylindole as a green oil:


Àε¹5gÀ» 10.8g ÀÇ koh¸¦ dmso10ml¿¡ ³ìÀÎ ¼Ö·ç¼Ç¿¡ Ãß°¡ÇÑ´Ù.

12.9ÀÇ 1-bromopentaneÀ» Ãß°¡ÇÏ°í ÁÖÀ§¿Âµµ¿¡ ¸ÂÃß¾î ±³¹ÝÇÏ°í

¹°·Î ³Ã°¢ÇÏ°í dcmÀ¸·Î ¼¼¹ø ÃßÃâÇÑ´Ù

ÀÌÈÄ mgso4·Î °ÇÁ¶ÇÑ´Ù..


·Î Áö½Ã¼­¸¦ Çؼ®Çߴµ¥ ÀÌ°ÍÀÌ À߸´ÂÁö ¿©·¯ºÐµé²² ¿©Âã°í½Í½À´Ï´Ù.

ÀÌÈÄ ÆÄ¿ì´õÇüÅ·Π°ÇÁ¶¸¦ ÇÏ°í½ÍÀºµ¥ ¾î¶»°Ô °ÇÁ¶ÇÏ¿© ÆÄ¿ì´õºÐ¸»À» 

¼öµæÇÒÁö¿¡ Á¶¾ðºÎŹµå¸³´Ï´Ù.

Crushed KOH´Â ÆÄ¿ì´õÇüŸ¦ ¸»Çϴ°Ͱ°Àºµ¥ ¸Â³ª¿ä?^^

ÇÕ¼º½Ã dmso¿ë¸Å¿¡ Á¶°¢µÈ koh¸¦ ³ìÀÌ´Ï Àß³ìÁö¾Ê³×¿ä.


½ºÅ×Æijë Stefano   13-01-29 21:16
(0) È­ÇÐ Àü°øÀڷμ­ koh mgso4 µîÀ¸·Î ¾²Áö ¸»¾Æ´Þ¶ó´Â ÁÖ¹®ÀÔ´Ï´Ù.  ¶Ç ¹Ýº¹ÇÏÁö¸¸ ±ÛÀ» ¾µ ¶§ ºÒÇÊ¿äÇÑ ºóÁÙÀº »ç¿ëÇÏÁö ¾Ê´Â °ÍÀÌ ÁÁ½À´Ï´Ù. 

(1) ¿ø¹®ÀÇ ³»¿ëÀº ´ÙÀ½°ú °°½À´Ï´Ù.  À̾߱Ⱑ ¾à°£ ºñ¾àµÈ °ÍÀº °ýÈ£( )¾È¿¡ º¸Ãæ¼³¸íÀ» °çµé¿´½À´Ï´Ù.

"10mLÀÇ DMSO¿¡ 5gÀÇ IndoleÀÌ µé¾îÀÖ´Â ¿ë¾×À» ±³¹ÝÇϸ鼭 10.8ÀÇ KOH ºÎ½º·¯±â¸¦ ³Ö¾îÁØ ´ÙÀ½,
N2ºÐÀ§±â¿¡¼­ 1.5½Ã°£µ¿¾È 12.9ÀÇ 1-Bromopentane(1-BP)À» °¡Çß´Ù.

¹°À» ºÎ¾î¼­ ¹ÝÀÀÀ» ÁßÁö½ÃÅ°°í È¥ÇÕ¹° ºÎÇÇÀÇ 3¹èÁ¤µµµÇ´Â DCMÀ¸·Î ÃßÃâÇÏ¿© (»óºÎ´Â ¹°Ãþ, ÇϺÎÀÇ) À¯±â¹°ÃþÀ» ¹Þ¾Æ³½ ÈÄ ÀÌ À¯±â¹°ÃþÀ» (¹«¼ö)MgSO4¸¦ ³Ö¾î °ÇÁ¶½ÃŲ( ´ÙÀ½ ¿©°úÁö·Î °É·¯³Â)´Ù. 

Kugelrohr Áõ¹ß±â¸¦ »ç¿ëÇÏ¿© °ÇÁ¶(ÀÜ·ù ¼öºÐÀÌ Á¦°Å)µÈ -NPI ¿ë¾×À» 200µµ 19 in-Hg Áø°ø(483 torr)»óÅ¿¡¼­ (DCMÀ») Áõ¹ßÇÑ ÈÄ 8.15g (¼øµµ98%)ÀÇ (¿¬)³ì»ö ±â¸§Çü»óÀÇ N-Pentylindole(NPI)°¡ ¾ò¾îÁ³´Ù." 
   
(2) Ʋ¸°Á¡µé
-KOH¸¦ DMSO¿¡ ³ìÀÎ °ÍÀÌ ¾Æ´Ï°í IndoleÀ» DMSO¿¡ ³ìÀΰ͠
-ambient temperature¸¦ Á÷¿ªÇϸé ÁÖÀ§(ÁÖº¯)¿ÂµµÀÌÁö¸¸ ¹ø¿ªÀº "»ó¿Â"À̶ó°í ÇØ¾ß ´õ ÀûÀýÇÔ.
-3 portions´Â ¼¼¹øÀ̶ó´Â ¶æÀ̶ó±â º¸´Ù´Â 3¹è (ºÎÇÇ)·Î ºÁ¾ß ÇÕ´Ï´Ù.

(3) °áÁ¤¼º Á¦Ç°
Á¦Ç°À» ÆÄ¿ì´õ ÇüÅ·Π°ÇÁ¶ÇÏ·Á¸é ¼øµµ°¡ ¾ÆÁÖ ³ô¾Æ¾ß Çϴµ¥ ¿©±â¼­´Â ¼øµµ°¡ ³ôÁö ¾Ê¾Æ¼­ Oil (±â¸§)»óÀÇ ¹°ÁúÀÌ ¾ò¾îÁø °ÍÀÔ´Ï´Ù.  98%°¡ ¼öÀ²ÀÎÁö ¼øµµÀÎÁö ÀοëÇÑ ¹®Àå¿¡¼­´Â ¾Ë ¼ö°¡ ¾øÁö¸¸  (ºÐÀÚ·®ÀÌ 187.28ÀÓÀ» °¨¾ÈÇÏ¸é ¼öÀ² 100%À̶ó°í Çصµ 8g Á¤µµ¹Û¿¡ »ý¼ºµÇÁö ¾ÊÀ» ÅÍÀ̹ǷÎ) ¼øµµ¸¦ ³ªÅ¸³¾  °¡¸Á¼ºÀÌ ³ô½À´Ï´Ù.  ÀÌ Oil»óÀÇ ¹°ÁúÀ» (Àç°áÁ¤¹æ¹ý µî)Àû´çÇÑ ¹æ¹ýÀ¸·Î  ´õ Á¤Á¦ÇÏ¸é ´õ ³ôÀº ¼øµµÀÇ °í»ó¹°ÁúÀ» ¾òÀ» ¼ö ÀÖÀ» °ÍÀÔ´Ï´Ù.   

(4) ¹ÝÀÀ ¹× ÈÄó¸® Á¶ÀÛ
Crushed KOH´Â FlakeÇü °íü ȤÀº °áÁ¤À» Àß°Ô ºÎ¼ø°ÍÀ̶ó°í º¾´Ï´Ù.  ¾Æ¸¶ ºÐ¸»Á¤µµ·Î ºÐ¼âÇÏ´Â °ÍÀÌ ¹ÝÀÀ¿¡ À¯¸®ÇÏ°ÚÁö¿ä.  KOH´Â DMSO¿¡´Â Àß ³ìÁö ¾Ê°ÚÁö¸¸ ù ¹ÝÀÀ¿¡ ÀÇÇØ ¼­¼­È÷ (Indole-KÈ­ÇÕ¹°·Î?) ¼Ò¸ðµÇÁö ¾Ê³ª »ý°¢µË´Ï´Ù. 

±×ÈÄ ÀÌ ¹°ÁúÀÌ 1-BP¿Í ¹ÝÀÀÇÏ¿© KBrÀÌ »ý¼ºµÇ¸é¼­ NPI°¡ ¾ò¾îÁö°í °ú·®ÀÇ KOH´Â DMSO¿Í ÇÔ²² ¹ÝÀÀÈÄ ½ñ¾Æ ºÎÀº ¹°¿¡³ì¾Æ ¼ö¿ëÃþ¿¡ ³²ÀÌ ÀÖ°Ô µÉ °ÍÀ¸·Î º¾´Ï´Ù. 

»ý¼ºµÈ NPI´Â DCMÀ¸·Î ÃßÃâÇÑ ´ÙÀ½ À¯±âÃþ¿¡ ÀÜ·ùÇÏ´Â ¹°¹æ¿ïÀ» ¿ÏÀüÈ÷ Á¦°ÅÇÏ°í ¿ëÁ¦DCMÀ» ³¯·Á¹ö¸®¸é NPI°¡ ³²°Ô µÉ °ÍÀÔ´Ï´Ù.
   

Copyright 1999.07.10-Now ChemEng.co.kr & 3D System Engineering. (mail : ykjang@naver.com, call 010-4456-8090)