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5Â¥2007-08-28 17:00:33
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In a typical experiment (1R)-(+)-camphor (7.61 g, 50 mmol) in dry THF (10 ml) was added dropwise to a magnetically stirred solution of t-BuOK (1.73 g, 60 mmol) in dry THF (15 ml) at -30¡ãC under nitrogen. The mixture was stirred at -30¡ãC for 10 rain., treated with i-AmONO (7.03 g, 60 mmol), and left at room temperature under stirring for 12hr. The solvent was distilled off, the residue diluted with water and extracted with Et20 to separate any neutral component. The aqueous part was acidified with cold HOAc and extracted with Et20 to afford the crude oxime as light yellow solid which on crystallisation (hexane - EtOH) afforded the desired oxime 9 (7.7 g, 85 %). ÕâÊÇÈ«ÎÄ ÄǸö°ïæ·ÒëÏÂi-AmONOÕâ¸ö´Ê Ôù½ð±Ò1¸ö... |

2Â¥2007-08-28 15:18:13













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