反応 #1251

反応方程式

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

溶媒

DMSO

反応条件

後処理

1. 1
   その他The excess bromopropane was then evaporated
2. 2
   その他The mixture was partitioned between water and ether
3. 3
   その他The aqueous layer was separated
4. 4
   抽出extracted with ether
5. 5
   洗浄The combined ether extracts were washed with water and brine
6. 6
   乾燥dried over Na2SO4
7. 7
   濃縮concentrated to an oil
8. 8
   その他The oil was purified through silica gel column chromatography

実験手順

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.

出典