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| General Procedure for Diastereoselective Alkyne Addition (2). Lithium hexamethyldisilazide (LiHMDS) (1 M in THF, 4.4 mmol, 4.0 eq) was dissolved in anhydrous hexanes (20 mL) at −78 ¡ãC, the appropriate alkyne (4.4 mmol, 4.0 eq) was added, and the reaction was removed from the cold bath and stirred for 10 min, then recooled to −78 ¡ãC. Vacuum-dried resin 1 (800 mg, 1.11 meq, 1.0 eq) was swollen with THF (20 mL) for 10 min, then cooled to −78 ¡ãC and the lithium acetylide solution was added via cannula. The reaction was allowed to warm to RT with stirring over 24 h. The reaction was quenched with water (100 mL), then the resin was washed and dried to afford propargyl sulfinamides 2. |
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- ×¢²á: 2009-10-29
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lgq101(½ð±Ò+20, ·ÒëEPI+1): лл~~~~~ 2011-08-20 08:44:25
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lgq101(½ð±Ò+20, ·ÒëEPI+1): лл~~~~~ 2011-08-20 08:44:25
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Diastereoselective Alkyne Ìí¼ÓµÄÒ»°ã¹ý³Ì£¨2£©£¬ Lithium hexamethyldisilazide (LiHMDS)£¨1 M in THF, 4.4 mmol, 4.0 eq£©ÔÚ−78 ¡ãCÈܽâÓÚÎÞË®¼ºÍéÖУ¬Ìí¼ÓÊÊÁ¿µÄȲÌþ(4.4 mmol, 4.0 eq)£¬·´Ó¦´Ó±ùÔ¡ÖÐÒÆ³ö²¢½Á°è10·ÖÖÓ£¬È»ºóÖØÐÂÀäÈ´µ½ −78 ¡ãC¡£Õæ¿Õ¸ÉÔïÊ÷Ö¬ (800 mg, 1.11 meq, 1.0 eq)ÓÃËÄÇâ߻ૠ(20 mL)½þÅÝ10·ÖÖÓ£¬È»ºóÀäÈ´µ½−78 ¡ãC ²¢Í¨¹ý²å¹Ü¼ÓÈëÒÒȲﮡ£Õû¸ö·´Ó¦Í¨¹ý½Á°è24СʱʹζȴﵽÊÒΡ£ÓÃË® (100 mL)´ã»ð·´Ó¦£¬È»ºóÏ´µÓ²¢¸ÉÔïÊ÷Ö¬À´¹ýÂËpropargyl sulfinamides 2¡£ ÄǼ¸¸ö»¯Ñ§ÊÔ¼Á²»ÖªµÀÔõô·Òë¡£ |
2Â¥2011-08-20 07:56:48
quzuoyin
ÖÁ×ðľ³æ (СÓÐÃûÆø)
- ·ÒëEPI: 16
- Ó¦Öú: 0 (Ó×¶ùÔ°)
- ½ð±Ò: 10547.6
- É¢½ð: 1502
- ºì»¨: 6
- Ìû×Ó: 149
- ÔÚÏß: 200.3Сʱ
- ³æºÅ: 887520
- ×¢²á: 2009-10-29
- רҵ: ¿¹Ö×ÁöÒ©ÎïÒ©Àí
3Â¥2011-08-20 08:03:28













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