反应 #1251

反应方程式

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

溶剂

DMSO

反应条件

后处理

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

实验过程

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.

来源