تفاعل #1251

معادلة التفاعل

product

N-Propyl-2,5-dimethyl-3-(2,4,6-trimethylphenyl)-2H-pyrazolo[4,3-d]pyrimidin-7-amine

KOH

1-bromopropane

→

title compound

N,N-Dipropyl-2,5-dimethyl-3-(2,4,6-trimethylphenyl)-2H-pyrazolo[4,3-d]pyrimidin-7-amine

المذيبات

DMSO

ظروف التفاعل

المعالجة

1. 1
   أخرىThe excess bromopropane was then evaporated
2. 2
   أخرىThe mixture was partitioned between water and ether
3. 3
   أخرىThe aqueous layer was separated
4. 4
   استخلاصextracted with ether
5. 5
   غسيلThe combined ether extracts were washed with water and brine
6. 6
   تجفيفdried over Na2SO4
7. 7
   تركيزconcentrated to an oil
8. 8
   أخرىThe oil was purified through silica gel column chromatography

الإجراء التجريبي

A mixture of the product of step F (400 mg, 1.2 mmol), powder KOH (1.0 g) and 1-bromopropane (1 mL) in 2 mL of DMSO was heated at 60° C. for 8 hours. The excess bromopropane was then evaporated. The mixture was partitioned between water and ether. The aqueous layer was separated and extracted with ether. The combined ether extracts were washed with water and brine, dried over Na2SO4 and concentrated to an oil. The oil was purified through silica gel column chromatography to give 260 mg of the title compound as an oil. 1H NMR (CDCl3): d 0.97 (t, 6H), 1.76 (m, 4H), 1.96 (s, 6H), 2.32 (s, 3H), 2.45 (s, 3H), 3.77 (s, 3H), 3.40-4.30 (br, 4H), 6.95 (s, 2H)ppm. The hydrochloride salt prepared in Ether/HCl melted at 210°-13° C.

المصدر