Реакция #1251

Уравнение реакции

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

Растворители

DMSO

Условия реакции

Обработка

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

Методика

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.

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