Glycol monoethyl ether → 5-[2-(2-Ethoxyethoxy)-5-(4-ethylpiperazin-1-ylsulphonyl)pyridin-3-yl]-3-ethyl-2-(pyridin-2-yl)methyl-2,6-dihydro-7h-pyrazolo[4,3-d]pyrimidin-7-one

A stirred mixture of potassium bis(trimethylsilyl)amide (434 mg, 2.2 mmol) and 2-ethoxyethanol (2 ml) was heated at 90° C. for 30 minutes, then allowed to cool. A solution of the title compound of Example 1 (153 mg, 0.27 mmol) in 2-ethoxyethanol (2 ml) was added and the reaction mixture stirred at 110° C. for 18 hours, then allowed to cool. The resulting mixture was evaporated under reduced pressure and the residual, brown oil purified by column chromatography on silica gel, using dichloromethane:methanol (95:5) as eluant, to furnish the title compound (110 mg, 68%) as a yellow foam. δ (CDCl3): 1.04 (3H, t), 1.31 (6H, m), 2.41 (2H, q), 2.54 (4H, m), 3.04 (2H, q), 3.14 (4H, m), 3.72 (2H, q), 3.90 (2H, t), 4.78 (2H, t), 5.67 (2H, s), 7.10 (1H, d), 7.22 (1H, m), 7.63 (1H, m), 8.57 (1H, d), 8.62 (1H, s), 8.99 (1H, s), 10.78 (1H, s). LRMS: m/z 597 (M+1)+.

1. temperatureto cool
2. temperatureto cool
3. customThe resulting mixture was evaporated under reduced pressure
4. customthe residual, brown oil purified by column chromatography on silica gel

ORDレコード

ord-8d7f89ca218a412ea69400354d7ae0ef

出典データセット

uspto-grants-2002_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06458951B2