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ÇëÄÄλ´óÏÀ¿´¹ýÀàËÆµÄÎÄÏ×£¬×ö¹ýÀàËÆµÄºÏ³É£¬°ï°ï棬ÊÇÔÚŪ²»Ã÷°×£¡ ºìÉ«²¿·ÖÊÇÖØµã£¬Âé·³Ïêϸ˵Ã÷һϣ¬µ½µ×¸ÃÔõô²Ù×÷£¬±ØÓÐÖØÐ»£¡ compound (3) was dissolved in dry 1,2-dibromoethane (2.4 mL, 27.6 mmol). Hexamethyldisilazane (3 mL, 13.8 mmol) was added to the solution, which was stirred at 120 ¡ãC for 20 h. The reaction mixture was cooled to room temperature, after which time EtOH (15 mL) was added, and the resulting solution was stirred at reflux temperature for 0.5 h. Following removal of the solvent in vacuo, the residue was dissolved into EtOAc (60 mL) and washed with water (3 x15 mL). The organic layer was dried over MgSO4 and evaporated to give 5 (2.4 g) containing ca. 50% 6 resulting from dehydrohalogenation of 5 in the presence of hexamethyldisilazane: 31P NMR (CDCl3) d 31.37, 38.97. This residue was treated with HC(OEt)3 (4.0 mL, 19.2 mmol) for 1.5 h at reflux temperature with simultaneous removal of resulting EtOH, following which excess HC(OEt)3 was removed in vacuo. The residue was subjected to silica gel chromatography (EtOAc/acetone 3:1) to give 7 (1.71 g, 57% over two steps) as a colorless oil: [ Last edited by dingbaiyu107 on 2010-11-27 at 10:24 ] |
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2Â¥2010-11-27 10:31:37
dingbaiyu107
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3Â¥2010-11-27 10:42:06
pl_zzu
Òø³æ (Ö°Òµ×÷¼Ò)
- ²©Ñ§EPI: 26
- Ó¦Öú: 15 (СѧÉú)
- ¹ó±ö: 2.45
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- ºì»¨: 20
- Ìû×Ó: 3700
- ÔÚÏß: 656.7Сʱ
- ³æºÅ: 1106643
- ×¢²á: 2010-09-24
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4Â¥2010-11-27 10:51:55
dingbaiyu107
ľ³æ (СÓÐÃûÆø)
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- Ìû×Ó: 278
- ÔÚÏß: 59.8Сʱ
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5Â¥2010-11-27 11:19:44













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