反应详情

To 4-[2-(dimethylamino)ethoxy]benzoic acid hydrochloride (66 mg, compound obtained in Reference example 78(2)) is added successively methylene chloride (2 mL), 1-(3-ethoxybenzyl)-4-piperazin-1-yl-1H-pyrazolo[3,4-d]pyrimidine dihydrochloride (100 mg), 1-hydroxybenzotriazole (49.3 mg), triethylamine (118.6 μL) and 1-ethyl-3-[3-(dimethylamino)propyl]carbodiimide hydrochloride (70 mg) and the mixture is stirred at room temperature for 17 hours. The reaction mixture is diluted with chloroform (5 mL) and thereto is added a saturated sodium hydrogencarbonate solution (10 mL). After stirring, the organic layer is separated and concentrated. The resultant crude product is purified by flash column chromatography on NH-silica gel (Solvent; ethyl acetate:chloroform=1:0→0:1) to give 1-(3-ethoxybenzyl)-4-[4-[4-[2-(dimethylamino)ethoxy]benzoyl]piperazin-1-yl]-1H-pyrazolo[3,4-d]pyrimidine (103 mg, yield; 69%) as an amorphous powder. MS (APCI) m/z: 530 [M+H]+

1. stirringAfter stirring
2. customthe organic layer is separated
3. concentrationconcentrated
4. customThe resultant crude product is purified by flash column chromatography on NH-silica gel (Solvent; ethyl acetate:chloroform=1:0→0:1)