Sodium sulfate decahydrate → HCID 89768198、化合物

To a mixture of ethyl 4-methyl-2-(trifluoromethyl)pyrimidine-5-carboxylate (122.4 mg) in toluene (5.1 mL) was added diisobutylaluminum hydride (1.0 mol/L in hexane, 1.150 mL) at 0° C. The mixture was stirred at 0° C. under nitrogen atmosphere for 2.5 h, and then at room temperature for 2 h. To the mixture was added diisobutylaluminum hydride (1.0 mol/L in hexane, 0.58 mL) again at 0° C. and the mixture was stirred at 0° C. for 2 h. To the mixture was added sodium sulfate decahydrate (556 mg), and the mixture was stirred at room temperature overnight. The mixture was filtered through on the pad of Celite®. The filtrate was concentrated in vacuo to give the title compound (97.6 mg).

1. waitat room temperature for 2 h
2. stirringthe mixture was stirred at 0° C. for 2 h
3. stirringthe mixture was stirred at room temperature overnight
4. filtrationThe mixture was filtered through on the pad of Celite®
5. concentrationThe filtrate was concentrated in vacuo

ORDレコード

ord-464c8003ef5d4dfa89dd122143c0839a

出典データセット

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09238639B2