content_image/897948.jpg content_image/897949.jpg content_image/897945.jpg content_image/897947.jpg content_image/897946.jpg
[0274] Synthesis of Intermediate J 

<img src='content_image/897948.jpg'>

<img src='content_image/897949.jpg'>

[0275] Intermediate I, 23.9 g, was dissolved in 100 g of acetonitrile. Under ice cooling, 4.91 g of diisopropylethyl› amine and 2.55 g of chloromethyl methyl ether were added 

## Example 1-2-3 

<img src='content_image/897945.jpg'>

to the solution, which was stirred at room temperature for 1 hour. The procedure of adding 4.91 g of diisopropylethyl› amine and 2.55 g of chloromethyl methyl ether to the solution under ice cooling, and stirring at room temperature for 1 hour was repeated 4 times. With stirring, the solution was aged overnight at room temperature. Deionized water, 120 g, was added to the solution to quench the reaction. This was followed by addition of 100 g of MIBK and stirring, whereupon an organic layer was taken out. The organic layer was washed 2 times with 10 wt % methanol aqueous solution, 3 times with saturated ammonium chloride aque› ous solution, and 3 times with 5 wt % methanol aqueous solution. The organic layer was concentrated under reduced pressure. Methylene chloride was added to the concentrate so as to form a 25 wt % solution, and 300 g of hexane was added for crystallization. The precipitate was collected by filtration, washed twice with hexane, and dried in vacuum, obtaining 21.9 g of the end compound, Intermediate J as solid (yield 82%). 

[0276] Intermediate J was analyzed by spectroscopy. The NMR spectra, $^{1}$H- and $^{19}$F-NMR in DMSO-d$_{6 }$ are shown in FIGS. 17 and 18. 

[0277] IR (D-ATR): 3390, 3045, 3019, 2975, 1589, 1492, 1463, 1417, 1339, 1305, 1258, 1240, 1221, 1185, 1153, 1105, 1080, 1003, 988, 968, 922, 844, 816, 730, 700, 649 cm- 1 

[0278] TOF-MS (MALDI): Positive M+ 761 

[0279] Synthesis of Intermediate K 

<img src='content_image/897947.jpg'>

[0280] A mixture of 12 g of Intermediate J, 5.5 g of Compound B, 60 g of MIBK, and 60 g of deionized water was stirred at room temperature, from which an organic 

## Example 1-2-4 

<img src='content_image/897946.jpg'>

