| ²é¿´: 489 | »Ø¸´: 1 | |||
| ±¾Ìû²úÉú 1 ¸ö ·ÒëEPI £¬µã»÷ÕâÀï½øÐв鿴 | |||
ÓÞÙâÙâгæ (³õÈëÎÄ̳)
|
[ÇóÖú]
Óлú·´Ó¦¹ý³Ì Ƭ¶Î·Òë
|
||
|
General procedure for the selective oxidation of suldes to sulfoxides To a mixture of various suldes (1 mmol) and DBUH-Br3 (0.1 mmol, 0.039 g) in CH3CN (15 mL), H2O2 30% (v/v)(1.4 mmol) was added gradually. After the completion of the reaction which was monitored by TLC using n-hexane:EtOAc (7:3), the solvent was removed and CH2Cl2 (20 mL) was added and the mixture was washed with water(15 mL), 5% HCl solution (15 mL) and water (15 mL), respectively. The organic phase was then dried over anhydrousNa2SO4 and the solvent was removed under reduced pressure. The resulting products were determined by their 1HNMR spectrums and compared with the authentic samples. The synthesis and X-ray structure of DBUH-Br3 as the catalyst have already been reported elsewhere (Fig. 1)[13].In order to get an insight into the optimum catalytic conditions for the selective oxidation of suldes to sulfoxides,the oxidation reaction of methylphenylsulde by hydrogen peroxide as a model experiment was studied at different temperatures and catalyst/H2O2 ratios. The results are summarized in Table 1. Different solvents were also screened. or the oxidation of methylphenylsulde, and as the result acetonitrile was found to be the best solvent in terms of activity and selectivity. |
» ²ÂÄãϲ»¶
ÇóbÇøÔºÐ£µ÷¼Á
ÒѾÓÐ5È˻ظ´
0854AI CV·½ÏòÕÐÊÕµ÷¼Á
ÒѾÓÐ4È˻ظ´
296Çóµ÷¼Á
ÒѾÓÐ7È˻ظ´
302Çóµ÷¼Á
ÒѾÓÐ4È˻ظ´
086000ÉúÎïÓëÒ½Ò©292Çóµ÷¼Á
ÒѾÓÐ5È˻ظ´
±±¿Æ281ѧ˶²ÄÁÏÇóµ÷¼Á
ÒѾÓÐ14È˻ظ´
²ÄÁÏÓ뻯¹¤ 322Çóµ÷¼Á
ÒѾÓÐ5È˻ظ´
333Çóµ÷¼Á
ÒѾÓÐ11È˻ظ´
²ÄÁÏר˶ 335 ·ÖÇóµ÷¼Á
ÒѾÓÐ3È˻ظ´
07»¯Ñ§303Çóµ÷¼Á
ÒѾÓÐ3È˻ظ´
8814402
ÖÁ×ðľ³æ (Ö°Òµ×÷¼Ò)
- ·ÒëEPI: 509
- Ó¦Öú: 18 (СѧÉú)
- ¹ó±ö: 0.381
- ½ð±Ò: 12916.1
- É¢½ð: 47
- ºì»¨: 16
- Ìû×Ó: 4183
- ÔÚÏß: 357.8Сʱ
- ³æºÅ: 1184404
- ×¢²á: 2011-01-06
- רҵ: Ò©ÎïѧÆäËû¿ÆÑ§ÎÊÌâ
¡¾´ð°¸¡¿Ó¦Öú»ØÌû
¡ï
sltmac(½ð±Ò+1): лл½»Á÷~~ 2011-05-30 18:56:52
ÓÞÙâÙâ(½ð±Ò+12, ·ÒëEPI+1): 2011-05-30 22:01:47
sltmac(½ð±Ò+1): лл½»Á÷~~ 2011-05-30 18:56:52
ÓÞÙâÙâ(½ð±Ò+12, ·ÒëEPI+1): 2011-05-30 22:01:47
|
General procedure for the selective oxidation of suldes to sulfoxides Ñ¡ÔñÐÔÑõ»¯suldesΪÑÇí¿µÄÒ»°ã²½Öè To a mixture of various suldes (1 mmol) and DBUH-Br3 (0.1 mmol, 0.039 g) in CH3CN (15 mL), H2O2 30% (v/v)(1.4 mmol) was added gradually. Ïòº¬Óв»Í¬suldes£¨1mmol£©ºÍDBUH-Br3 (0.1 mmol, 0.039 g)»ìºÏÎïµÄ15mL CH3CN ÖÐÖ𽥵ؼÓÈë30%(v/v)¹ýÑõ»¯Çâ(1.4 mmol)¡£After the completion of the reaction which was monitored by TLC using n-hexane:EtOAc (7:3), the solvent was removed and CH2Cl2 (20 mL) was added and the mixture was washed with water(15 mL), 5% HCl solution (15 mL) and water (15 mL), respectively. ·´Ó¦ÍêÈ«£¨Í¨¹ýÕý¼ºÍ飺ÒÒËáÒÒõ¥7:3±¡²ãÉ«Æ×¼à²â£©ºó£¬ÒƳýÈܼÁ£¬¼ÓÈë20mL¶þÂȼ×Í飬»ìºÏÒºÏȺó·Ö±ðÒÔ15mLË®¡¢15mL5%HClºÍ15mLË®ÇåÏ´¡£The organic phase was then dried over anhydrousNa2SO4 and the solvent was removed under reduced pressure. ÓлúÏàËæºóÒÔÎÞË®ÁòËáÄÆ¸ÉÔï²¢¼õѹ³ýÈ¥ÈܼÁ¡£The resulting products were determined by their 1HNMR spectrums and compared with the authentic samples.²úÎïÒÔÇâÆ×¼ø¶¨²¢ºÍ¿ÉÐÅÑùÆ·¶ÔÕÕ¡£ The synthesis and X-ray structure of DBUH-Br3 as the catalyst have already been reported elsewhere (Fig. 1)[13].×÷Ϊ´ß»¯¼ÁµÄDBUH-Br3µÄºÏ³ÉºÍXÉäÏßÑÜÉä½á¹¹ÒÑÓб¨µÀ£¨Í¼1£©¡£In order to get an insight into the optimum catalytic conditions for the selective oxidation of suldes to sulfoxides,the oxidation reaction of methylphenylsulde by hydrogen peroxide as a model experiment was studied at different temperatures and catalyst/H2O2 ratios. ΪÁË»ñµÃÑ¡ÔñÐÔÑõ»¯suldesΪÑÇí¿µÄ×î¼Ñ´ß»¯Ìõ¼þ£¬ÔÚ²»Í¬µÄζȺʹ߻¯¼Á/¹ýÑõ»¯Çâ±ÈÌõ¼þÏ£¬Ñо¿ÁË×÷Ϊģʽ·´Ó¦µÄmethylphenylsulde ±»¹ýÑõ»¯ÇâÑõ»¯µÄ·´Ó¦¡£The results are summarized in Table 1.½á¹û×ܽáÔÚ±í1ÖС£ Different solvents were also screened. ²»Í¬µÄÈܼÁÒ²½øÐÐÁËɸѡ¡£For the oxidation of methylphenylsulde, and as the result acetonitrile was found to be the best solvent in terms of activity and selectivity.¶ÔmethylphenylsuldeµÄÑõ»¯£¬´Ó½á¹ûÀ´¿´£¬ÒÒëæ¾Í·´Ó¦»îÐÔºÍÑ¡ÔñÐÔ¶øÑÔÊÇ×î¼ÑÈܼÁ¡£ |
2Â¥2011-05-30 09:02:47













»Ø¸´´ËÂ¥