| ²é¿´: 1394 | »Ø¸´: 2 | ||
liuqifa½ð³æ (ÖøÃûдÊÖ)
|
[ÇóÖú]
Çó°ïæ·ÒëÒ»¶ÎÖÐÎÄÖÁÓ¢ÎÄ£¬Ð»Ð»£¡ ÒÑÓÐ1È˲ÎÓë
|
|
ÖØ½á¾§£º½«227.3gÎö¾§Â˱ý¼ÓÈëµ½2L¸ÉÔïµÄËÄ¿ÚÉÕÆ¿ÖУ¬¼ÓÈë454.6gTHF£¬ÉýÎÂÖÁ60-65¡æ£¬Ê¹¹ÌÌåÍêÈ«Èܽ⣬±£ÎÂ10min£¬ºó½µÎÂÖÁ50¡æÓý¾§1h£¬½µÎÂÖÁ-15~ -10¡æ±£ÎÂ1h£¬¹ýÂ˵ÃÂ˱ý219.12g£¬HPLC´¿¶È99.3%¡£ÂËÒº450.7g£¬ÂËÒº»ØÊÕTHFºóÁóµ×ÓÃÓÚÎö¾§Ì×ÓᣠÓÈÆäÊÇ¡°Óý¾§¡±ÒªÇó·Òë׼ȷ¡£Ð»Ð»£¡ |
» ²ÂÄãϲ»¶
¿¼Ñе÷¼Á
ÒѾÓÐ15È˻ظ´
Ò»Ö¾Ô¸2110£¬»¯Ñ§Ñ§Ë¶310·Ö£¬±¾¿ÆÖصãË«·ÇÇóµ÷¼Á
ÒѾÓÐ17È˻ظ´
282£¬Çóµ÷¼Á
ÒѾÓÐ8È˻ظ´
»¯Ñ§¹¤³Ìµ÷¼Á289
ÒѾÓÐ47È˻ظ´
297Çóµ÷¼Á
ÒѾÓÐ8È˻ظ´
»úеר˶270Çóµ÷¼Á£¬½ÓÊÜ¿çרҵ
ÒѾÓÐ4È˻ظ´
»¹Óл¯¹¤¶þÂÖµ÷¼ÁµÄѧУÂð
ÒѾÓÐ37È˻ظ´
22408µ÷¼ÁÇóÖú
ÒѾÓÐ5È˻ظ´
»¯¹¤µ÷¼ÁÇóµ¼Ê¦ÊÕÁô£¡Ò»Ö¾Ô¸Ê§Àû£¬Ì¤Êµ¿Ï¸É£¬ÓÐÖ²ÎïÌáÈ¡¿ÆÑоÀú
ÒѾÓÐ7È˻ظ´
²ÄÁϹ¤³Ì302·ÖÇóµ÷¼Á
ÒѾÓÐ14È˻ظ´
» ±¾Ö÷ÌâÏà¹Ø¼ÛÖµÌùÍÆ¼ö£¬¶ÔÄúͬÑùÓаïÖú:
ÇóÓ¢Óï´óÉñ·Òë
ÒѾÓÐ6È˻ظ´
ÇóÕâÁ½¸ö²Î¿¼ÎÄÏ×µÄÓ¢ÎÄ·Ò룬×îºÃ²»Òª°Ù¶È¡¢GoogleµÈ·ÒëÆ÷µÄÓ¢ÎÄ·Òë¡£
ÒѾÓÐ12È˻ظ´
±à¼À´ÐÅ£¬²»¶®£¬Çó´óÏÀ°ïæ·Ò룡
ÒѾÓÐ8È˻ظ´
רҵӢÓï·Òë¼±Óã¬Ð»Ð»´ó¼Ò~
ÒѾÓÐ3È˻ظ´
ºË´ÅÓ¢ÎÄÊý¾ÝÇó·Ò룡£¡£¡
ÒѾÓÐ3È˻ظ´
Çó·Òë Ò»¾ä»°
ÒѾÓÐ9È˻ظ´
ººÓï·Òë³ÉÓ¢ÎÄ£¬Çë¸÷λ³æÓѰïæ·ÒëÒ»ÏÂлл
ÒѾÓÐ1È˻ظ´
Õâ¾ä»°ÓÐЩ³¤£¬ºó°ë¾ä·Ò벻̫ͨ˳£¬ÄÄλ°ïæ·Òëһϣ¿£¿£¿
ÒѾÓÐ19È˻ظ´
Çë½Ì´óÉñ£¬¿´¿´ÎÒ·ÒëµÄÈçºÎ£¬ÖÐÎÄ·Òë³ÉÓ¢ÎÄ
ÒѾÓÐ9È˻ظ´
ÇóÖúÖÐÎÄÕªÒª·Òë³ÉÓ¢ÎÄ¡£¡£¡£
ÒѾÓÐ12È˻ظ´
Ç뽫ÖÐÎÄÕªÒª·Òë³ÉÓ¢ÎÄ£¨Ã¿ÈË100½ð±Ò£¬Òª´ïµ½Ò»¶¨Ë®×¼£©
ÒѾÓÐ7È˻ظ´
ÇóÖú·ÒëÒ»¶ÎÓ¢ÎÄ
ÒѾÓÐ1È˻ظ´
Çó¸ßÊÖ°ïæ¿´Ò»¶ÎÓ¢ÎÄ£¬Éæ¼°µ½Êý¾Ý·ÖÎöÎÊÌ⣬ÈçÄܸø³ö˵µÃͨµÄÈ«ÎÄ·ÒëÁíÓÐ50BBÏàÔù
ÒѾÓÐ5È˻ظ´
Ò»¶ÎÓ¢ÎÄ·Òë³ÉÖÐÎÄ Ôõô¶Ï¾ä
ÒѾÓÐ2È˻ظ´
ÇóÒ»¾äÓ¢ÓïµÄ·Ò룬50¸ö½ð±Ò лл
ÒѾÓÐ8È˻ظ´
ÇëÇó°ïæ·ÒëÒ»¸öÖÐÎÄժҪΪӢÎÄ
ÒѾÓÐ3È˻ظ´
ÓлúʵÑé¹ý³Ì£¬ÇóÓ¢ÎÄ·Ò룬´óÉñÃǸϽôÀ´¿´¿´°¡
ÒѾÓÐ8È˻ظ´
Ó¢Óï²»ºÃÇó°ïÖú·Òë
ÒѾÓÐ12È˻ظ´
дÍêÖÐÎÄ·Ò룬»¹ÊÇÖ±½ÓдӢÎÄ
ÒѾÓÐ30È˻ظ´
ÐüÉÍ50½ð±Ò£¡£¡£¡ÇóÖú£¡·ÒëÒ»¶Î·´ÏàÉ«Æ×ÓëÖÊÆ×Ó¢ÎIJÙ×÷²½Öè
ÒѾÓÐ6È˻ظ´
Çó´óÏÀÃǰïæ·ÒëÒ»¶ÎÎÄ×Ö£¨ººÓï·Òë³ÉÓ¢Ó
ÒѾÓÐ5È˻ظ´
Çó¸ßÊÖ°ïæ·ÒëÒ»¶ÎÓ¢ÎÄ£¬ÒªÍ¨Ë³£¬²»Òª¹È¸è·ÒëÖ®ÀàµÄ£¡
ÒѾÓÐ3È˻ظ´
¡¾ÇóÖú¡¿50½ð±ÒÇóÖú·ÒëÒ»¾äÓ¢ÎÄ£¬¿É¼Ó½ð±Ò
ÒѾÓÐ3È˻ظ´
genhunter
ÖÁ×ðľ³æ (ÖøÃûдÊÖ)
- Ó¦Öú: 259 (´óѧÉú)
- ½ð±Ò: 9757.4
- É¢½ð: 10
- ºì»¨: 60
- Ìû×Ó: 2484
- ÔÚÏß: 1793Сʱ
- ³æºÅ: 2558361
- ×¢²á: 2013-07-22
- רҵ: Ö×Áö»¯Ñ§Ò©ÎïÖÎÁÆ
¡¾´ð°¸¡¿Ó¦Öú»ØÌû
¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï ¡ï
¸Ðл²ÎÓ룬ӦÖúÖ¸Êý +1
liuqifa: ½ð±Ò+10, ¡ïÓаïÖú 2015-02-28 11:44:12
¸Ðл²ÎÓ룬ӦÖúÖ¸Êý +1
liuqifa: ½ð±Ò+10, ¡ïÓаïÖú 2015-02-28 11:44:12
|
ÖØ½á¾§£º½«227.3gÎö¾§Â˱ý¼ÓÈëµ½2L¸ÉÔïµÄËÄ¿ÚÉÕÆ¿ÖУ¬¼ÓÈë454.6gTHF£¬ÉýÎÂÖÁ60-65¡æ£¬Ê¹¹ÌÌåÍêÈ«Èܽ⣬±£ÎÂ10min£¬ºó½µÎÂÖÁ50¡æÓý¾§1h£¬½µÎÂÖÁ-15~ -10¡æ±£ÎÂ1h£¬¹ýÂ˵ÃÂ˱ý219.12g£¬HPLC´¿¶È99.3%¡£ÂËÒº450.7g£¬ÂËÒº»ØÊÕTHFºóÁóµ×ÓÃÓÚÎö¾§Ì×ÓᣠRecrystalization: Add 227.3 g of filtration cake to a 2L dry flask with 4 necks to which 454.6g THF was then charged, temperature was then raised to 60-65¡æ to completely dissolve the solid. The temperature was kept at that range for 10 min, then lowered to 50¡æ for 1hr to start crystalization, after which, the temperature was lowered to -15~-10 ¡æ for 1 hr. After filtration, 219.12g cake was obtained, the purity was 99.3% as measured by HPLC. Also obtained was 450.7g filtrate, which after the recovery of THF, can be used as seeds for future crystalization process. |

2Â¥2015-02-27 23:57:20
![]() |
3Â¥2015-03-05 20:26:20













»Ø¸´´ËÂ¥

5