Beta-Alanine → HCID 75038129、化合物

To a mixture of 2-(5-oxo-2-thioxoimidazolidin-1-yl)-3-phenylpropanoic acid (0.100 g, 0.378 mmol) and 5-(4-bromophenyl)thiophene-2-carbaldehyde (0.101 g, 0.378 mmol) in acetic acid 5 mL is added β-alanine (3.37 mg, 0.038 mmol) and heat to 170° C. for 30 min under microwave irradiation. The resulting reaction mixture is cooled down and the solvent is removed. The pure product (0.120 g, 0.234 mmol, red solid) is obtained by column chromatography using MeOH/DCM, 2-7% ration solvent system. 1H-NMR (CD3OD/300 MHz): 7.84 (m, 1H), 7.63 (m, 1H), 7.50 (m, 3H), 7.15 (m, 6H), 6.69 (s, 1H), 5.66 (dd, J=11.4, 5.1 Hz, 1H), 3.69 (dd, J=14.4, 12.0 Hz, 1H), 3.51 (dd, J=10.5, 5.1 Hz, 1H). MS (ES+, m/z): 511.3 (M−−1, 100.0).

1. customThe resulting reaction mixture
2. temperatureis cooled down
3. customthe solvent is removed
4. customThe pure product (0.120 g, 0.234 mmol, red solid) is obtained by column chromatography

ORDレコード

ord-563c2ae96a264e4888149bbd27db5d7d

出典データセット

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08759384B2