تفاعل #1854077

معادلة التفاعل

allyl 4-chloro-4-oxobutyl succinate

4-[(1E,3E)-4-[trans-5-[[(1R,2R)-2-(2,4-difluorophenyl)-2-hydroxy-1-methyl-3-(1H-1,2,4-triazol-1-yl)propyl]thio]-1,3-dioxan-2-yl]-1,3-butadienyl]-3-fluorobenzonitrile

sodium hydride

→

title compound

المردود 40.0%

Allyl 4-[(1R,2R)-2-[[trans-2-[(1E,3E)-4-(4-cyano-2-fluorophenyl)-1,3-butadienyl]-1,3-dioxan-5-yl]thio]-1-(2,4-difluorophenyl)-1-[(1H-1,2,4-triazol-1-yl)methyl]propoxy]-4-oxobutyl succinate

المردود 40.0%

ظروف التفاعل

المعالجة

1. 1
   أخرىThe obtained crude title compound
2. 2
   أخرىwas purified by recycle preparative HPLC [LC-908; Japan Analytical Industry Co., Ltd.; GPC column JAIGEL-1H (20 mm i.d.×600 mm) and JAIGEL-2H (20 mm i.d.×600 mm) connected in series for use; solvent, chloroform]

الإجراء التجريبي

The crude allyl 4-chloro-4-oxobutyl succinate was treated with 4-[(1E,3E)-4-[trans-5-[[(1R,2R)-2-(2,4-difluorophenyl)-2-hydroxy-1-methyl-3-(1H-1,2,4-triazol-1-yl)propyl]thio]-1,3-dioxan-2-yl]-1,3-butadienyl]-3-fluorobenzonitrile (814 mg, 1.50 mmol) described in Reference example 1 and sodium hydride (55% dispersion in mineral oil; 70 mg, 1.6 mmol) according to a similar procedure to that described in Example 13-(2). The obtained crude title compound was purified by recycle preparative HPLC [LC-908; Japan Analytical Industry Co., Ltd.; GPC column JAIGEL-1H (20 mm i.d.×600 mm) and JAIGEL-2H (20 mm i.d.×600 mm) connected in series for use; solvent, chloroform] to afford the title compound (459 mg, 40% yield) as a colorless viscous material.

المصدر