Triethylamine → HCID 59333685、化合物

1-Hydroxybenzotriazole (31:3 mg, 0.23 mmol), N,N′-dicyclohexylcarbodiimide (71.6 mg, 0.35 mmol), and triethylamine (64.5 μl, 0.46 mmol) were added to an N,N-dimethylformamide solution (3.0 ml) of 5-{9-(cyclopropylmethyl)-8-[(3S)-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9H-purin-2-yl}pyrimidin-2-amine (115.6 mg, 0.26 mmol) and D-lactic acid (25.3 mg, 0.28 mmol) at room temperature. The resulting mixture was stirred for 18.5 hours followed by the addition of N,N′-dicyclohexylcarbodiimide (71.6 mg, 0.35 mmol) and the resulting mixture was stirred at 40° C. for 22 hours. 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 (68.7 mg, 57%) as a pale yellow solid.

1. stirringthe resulting mixture was stirred at 40° C. for 22 hours
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-33d1284552d4406eb6a8c71e3fb4ebf5

出典データセット

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08309546B2