Triethylamine → HCID 45376367、化合物

L-Lactic acid (48.2 μl, 0.55 mmol), 1-hydroxybenzotriazole monohydrate (42.0 mg, 0.27 mmol), 1-(dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (105.1 mg, 0.55 mmol), and triethylamine (76.4 μl, 0.55 mmol) were added to a methylene chloride (3.0 ml)-N,N-dimethylformamide (3.0 ml) mixture solution of 5-{8-[(3R)-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine (131.1 mg, 0.27 mmol) at room temperature. The resulting mixture was stirred for 5 days followed by the addition of L-lactic acid (48.2 μl, 0.55 mmol), 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (105.1 mg, 0.55 mmol), and triethylamine (76.4 μl, 0.55 mmol). The resulting mixture was stirred for 1 day and then the reaction mixture was poured into methylene chloride-methanol (10:1), washed with saturated aqueous sodium hydrogen carbonate solution, and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure and the resulting residue was purified by preparative thin layer silica gel chromatography (methylene chloride:methanol=10:1) to give the title compound (53.9 mg, 36%) as a pale yellow solid.

1. stirringThe resulting mixture was stirred for 1 day
2. washwashed with saturated aqueous sodium hydrogen carbonate solution
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationAfter filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. customthe resulting residue was purified by preparative thin layer silica gel chromatography (methylene chloride:methanol=10:1)

ORDレコード

ord-ef9c3ed771324eee9fdfe9da6c5f7036

出典データセット

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08309546B2