تفاعل #351397

معادلة التفاعل

6-fluoro-3-(4-piperidinyl)-1,2-benzisothiazole

1-[4-(3-chloropropoxy)-3-hydroxyphenyl]ethanone

NaHCO3

CH3CN

→

dark solid

المردود 97.0%

1-[4-[3-[4-(6-Fluoro-1,2-benzisothiazol-3-yl)-1-piperidinyl]propoxy]-3-hydroxyphenyl]ethanone

المردود 97.0%

المذيبات

H2O

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux under N2 for 65 hours
2. 2
   أخرىThe cooled reaction
3. 3
   استخلاصthe aqueous mixture was extracted with EtOAc
4. 4
   استخلاصThe EtOAc extract
5. 5
   غسيلwas washed with H2O (1×) and brine (3×)
6. 6
   تجفيفafter drying with MgSO4 the solvent
7. 7
   أخرىwas evaporated

الإجراء التجريبي

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisothiazole (2.4 g, 10.1 mmol), 1-[4-(3-chloropropoxy)-3-hydroxyphenyl]ethanone (2.5 g, 11.1 mmol), NaHCO3, (0.94 g, 11.1 mmol), KI (100 mg) and CH3CN (100 ml) was stirred at reflux under N2 for 65 hours. The cooled reaction was poured into H2O and the aqueous mixture was extracted with EtOAc. The EtOAc extract was washed with H2O (1×) and brine (3×) and after drying with MgSO4 the solvent was evaporated to give 4.2 g of a dark solid. Three consecutive recrystallizations from EtOH provided 2.1 g (48%) of glittery beige crystals m.p.=135°-137° C.

المصدر