تفاعل #1605839

معادلة التفاعل

hexyl chloroformate

dehydro-aripiprazole

potassium tert-butoxide

2-methyltetrahydrofuran

→

7-(4-(4-(2,3-dichlorophenyl)piperazin-1-yl)butoxy)quinolin-2-yl hexyl carbonate

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGstirred for a further 4 h
2. 2
   استخلاصextracted with ethyl acetate
3. 3
   تجفيفThe organic phase was dried over MgSO4
4. 4
   ترشيحfiltered
5. 5
   أخرىevaporated
6. 6
   أخرىThe residue was further purified on silica eluting with ethyl acetate/tetrahydrofuran
7. 7
   workup.ADDITIONthe major product containing fractions
8. 8
   أخرىevaporated
9. 9
   أخرىto give a yellow solid
10. 10
    أخرىThis was triturated in heptane (30 mL) for 2.5 h
11. 11
    ترشيحfiltered
12. 12
    أخرىdried
13. 13
    أخرىto give Compound-328 (1.55 g) as a white solid

الإجراء التجريبي

To a mixture of dehydro-aripiprazole (1.5 g, 3.4 mmol), potassium tert-butoxide (0.75 g, 6.7 mmol) and 2-methyltetrahydrofuran (30 mL) at 0° C. was added hexyl chloroformate (1.32 mL, 8.1 mmol). The reaction mixture was stirred for 2 h, allowed to self warm to room temperature and stirred for a further 4 h. The reaction mixture was then diluted with water and extracted with ethyl acetate. The organic phase was dried over MgSO4, filtered and evaporated. The residue was further purified on silica eluting with ethyl acetate/tetrahydrofuran and the major product containing fractions evaporated to give a yellow solid. This was triturated in heptane (30 mL) for 2.5 h, filtered and dried to give Compound-328 (1.55 g) as a white solid.

المصدر