| ²é¿´: 893 | »Ø¸´: 1 | ||
| ±¾Ìû²úÉú 1 ¸ö ·ÒëEPI £¬µã»÷ÕâÀï½øÐв鿴 | ||
yidiniaorenͳæ (ÕýʽдÊÖ)
|
[ÇóÖú]
Çó·Òë2¶Î»°£¬Ó¢Ò뺺£¬¹ØÓÚÈýÂÈÕáÌÇ-6-ÒÒËáõ¥ºÏ³É·½ÃæµÄ¡£
|
|
|
The method comprises (1) mixing chlorinating agent with chloroethane at a mass ratio of 1:2-4, cooling to 0C; (2) dropping sucrose 6-acetate-DMF mixed soln.(1:1-3, W/W) at -15-10C; (3) incubating at 0-100C for 2-6 times each for 0.5-2 h, heating to 110-115C, incubating for 1-4 h; (4) cooling to 0C, adding 20% alk. soln. to adjust pH to 9, neutralizing with HCl, vaporizing solvent, dissolving in water, filtering, extg. with Et acetate, dissolving in water, cooling to 20C for crystg. to obtain sucralose 6-acetate. Chlorinating agent is thionyl chloride, phosgene, oxalyl chloride, bis(trichloromethyl)carbonate and/or phosphorus trichloride. Chloroethane is 1,1,2-trichloroethane, 1,1,1-trichloroethane or 1,1,2,2-tetrachloroethane. The method has advantages of low DMF consumption, low cost, reduced side reaction, simple process, high yield(enhanced by 20% compared with that using DMF as solvent). The title method comprises dropping chlorinating agent I into mixed solvent, dropping sucrose-6-acetate/DMF soln., slowly heating, refluxing for 2h, adding chlorinating agent II/ethyl acetate or dichloroethane soln., further chlorinating at 110C, cooling, neutralizing with alkali, filtering, vacuum concg., dissolving in water under heating, extg., and vacuum removing solvent to obtain sucralose-6-acetate. The mixed solvent contains DMF and Et acetate or dichloroethane. The chlorinating agent I is thionyl chloride, phosphorus trichloride, phosphorus pentachloride or phosphorus oxychloride. The chlorinating agent II is trichloromethyl chloroformate or bis(trichloromethyl) carbonate. The method has advantages of easy operation, good selectivity of chlorination and high yield. |
» ²ÂÄãϲ»¶
²ÄÁÏ¿¼ÑÐÇóµ÷¼Á×Ü·Ö280
ÒѾÓÐ3È˻ظ´
Çóµ÷¼Á
ÒѾÓÐ4È˻ظ´
²ÄÁϵ÷¼Á
ÒѾÓÐ10È˻ظ´
Çóµ÷¼Áµ½²ÄÁÏ
ÒѾÓÐ3È˻ظ´
»¯¹¤Çóµ÷¼Á£¡
ÒѾÓÐ9È˻ظ´
301Çóµ÷¼Á
ÒѾÓÐ13È˻ظ´
308Çóµ÷¼Á
ÒѾÓÐ13È˻ظ´
²ÄÁϹ¤³Ì310ר˶µ÷¼Á
ÒѾÓÐ15È˻ظ´
304Çóµ÷¼Á
ÒѾÓÐ9È˻ظ´
081700£¬311£¬Çóµ÷¼Á
ÒѾÓÐ16È˻ظ´

anthappy
ľ³æ (ÖøÃûдÊÖ)
- ·ÒëEPI: 1
- Ó¦Öú: 4 (Ó×¶ùÔ°)
- ½ð±Ò: 4861.6
- ºì»¨: 6
- Ìû×Ó: 1791
- ÔÚÏß: 310.2Сʱ
- ³æºÅ: 272314
- ×¢²á: 2006-08-13
- ÐÔ±ð: MM
- רҵ: ¹âÆ×·ÖÎö
¡¾´ð°¸¡¿Ó¦Öú»ØÌû
¡ï ¡ï
°®ÓëÓêÏÂ(½ð±Ò+2): ¸ÐлӦÖú£¬»¶Ó³£À´£¡ 2011-08-22 08:45:58
yidiniaoren(½ð±Ò+80, ·ÒëEPI+1): лл~~Ã²ËÆÎÒÈý¸öÌû×Ó¶¼ÊÇÄã·ÒëµÄ°¡£¬Ì«¸ÐлÁË 2011-08-22 12:28:44
°®ÓëÓêÏÂ(½ð±Ò+2): ¸ÐлӦÖú£¬»¶Ó³£À´£¡ 2011-08-22 08:45:58
yidiniaoren(½ð±Ò+80, ·ÒëEPI+1): лл~~Ã²ËÆÎÒÈý¸öÌû×Ó¶¼ÊÇÄã·ÒëµÄ°¡£¬Ì«¸ÐлÁË 2011-08-22 12:28:44
|
¸Ã·½·¨°üÀ¨£º£¨1£©ÓëÂÈÒÒÍé»ìºÏÂÈ»¯¼ÁµÄÖÊÁ¿±ÈΪ1:2-4£¬ÀäÈ´µ½0C£¬£¨2£©ÔÚ-15-10CÌõ¼þϵÎÈë ÕáÌÇ 6 ¨CÒÒËá-DMF»ìºÏÒº£¨1:1-3£¬W/ W£©£¬£¨3£©ÔÚ0-100C·õ»¯2-6´Î£¬Ã¿´Î0.5-2 h£¬¼ÓÈȵ½110-115C£¬ÅàÓý1-4 h;£¨4 £©ÀäÈ´µ½0C£¬¼ÓÈë 20£¥¼îÐÔÈÜÒº£¬µ÷½ÚpHÖÁ9£¬ÓÃHClÖкͣ¬Õô·¢ÈܼÁ£¬ÔÚË®ÖÐÈܽ⣬¹ýÂË£¬ÓÃÒÒËáÒÒõ¥extg£¨ÝÍÈ¡£¿£©£¬ÈÜÓÚË®£¬ÀäÈ´µ½20CÓÃÓÚcrystg£¨½á¾§£¿£©¡£»ñµÃÈýÂÈÕáÌÇ6 - ´×Ëᣨsucralose 6-acetate£©¡£ÂÈ»¯¼ÁÊÇÑÇÁòõ£ÂÈ£¬¹âÆø£¬²Ýõ£ÂÈ£¬Ë«£¨ÈýÂȼ׻ù£©Ì¼Ëáõ¥ºÍ/»òÈýÂÈ»¯Áס£ÂÈÒÒÍéÊÇ1,1,2 - ÈýÂÈÒÒÍ飬1,1,1 - ÈýÂÈÒÒÍ飬1,1,2,2 - ËÄÂÈÒÒÍé¡£¸Ã·½·¨¾ßÓÐDMFÏûºÄµÍ£¬³É±¾µÍ£¬¸±·´Ó¦ÉÙ£¬¹¤ÒÕ¼òµ¥£¬²úÁ¿¸ß£¨ÓëʹÓöþ¼×»ù¼×õ£°·£¨DMF?£©ÎªÈܼÁÏà±È£¬Ìá¸ß20£¥£© Ö÷Òª·½·¨°üÀ¨µÎ¼ÓÂÈ»¯¼ÁIµ½»ìºÏÈÜÈÜÒº£¬µÎ¼Ó ÕáÌÇ-6-ÒÒËá/DMF soln£¬»ºÂý¼ÓÈÈ£¬»ØÁ÷2h£¬¼ÓÈëÂÈ»¯¼ÁII/ÒÒËáÒÒõ¥»ò¶þÂÈÒÒÍésoln£¬½øÒ»²½ÔÚ110¡æÂÈ»¯£¬ÀäÈ´£¬ÓüîÖкͣ¬¹ýÂË£¬Õæ¿Õconcg£¨Å¨Ëõ£¿£©£¬¼ÓÈÈÌõ¼þÏÂÈÜÓÚË®£¬extg£¨ÝÍÈ¡£¿£©£¬Õæ¿ÕÏû³ýÈܼÁ£¬»ñµÃÕáÌÇËØ-6-´×Ëᣨsucralose-6-acetate£©¡£»ìºÏÈܼÁÖк¬ÓÐDMFºÍ»ò¶þÂÈÒÒÍé¡£ÂÈ»¯¼ÁIÊÇÑÇÁòõ£ÂÈ£¬ÈýÂÈ»¯Á×£¬ÎåÂÈ»¯Á×»òÈýÂÈÑõÁס£ÂÈ»¯¼ÁIIÊÇÈýÂȼ׻ùÂȼ×Ëá»òË«£¨ÈýÂȼ׻ù£©Ì¼Ëáõ¥¡£¸Ã·½·¨¾ßÓвÙ×÷¼ò±ã£¬ÂÈ»¯Ñ¡ÔñÈÝÒ׺ͲúÁ¿¸ßµÄÓŵ㡣 |
2Â¥2011-08-22 07:01:57














»Ø¸´´ËÂ¥