Beta-Alanine → HCID 76698629, 화합물

To a mixture of 2-(5-oxo-2-thioxoimidazolidin-1-yl)-3-phenylpropanoic acid (0.055 g, 0.207 mmol) and 5-(3,4-dichloro-phenyl)thiophene-2-carbaldehyde (0.050 g, 0.207 mmol) in acetic acid 5 mL is added β-alanine (1.8 mg, 0.021 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 (0.060 g, 0.123 mmol, red solid) is obtained by column chromatography using MeOH/DCM, 2-7% ration solvent system. 1H-NMR (CDCl3/CD3OD/300 MHz): 7.84 (d, J=2.1 Hz, 1H), 7.60 (dd, J=8.7, 2.4 Hz, 1H), 7.44 (d, J=2.7 Hz, 1H), 7.17 (m, 6H), 6.85 (m, 1H), 6.42 (s, 1H), 5.61 (dd, J=11.1, 5.4 Hz, 1H), 3.66 (m, 1H), 3.53 (m, 1H). MS (ES−, m/z): 585.3 (M−, 100.0).

1. customThe resulting reaction mixture
2. temperatureis cooled down
3. customthe solvent is removed
4. customThe pure product (0.060 g, 0.123 mmol, red solid) is obtained by column chromatography

ORD 기록

ord-6e752bc0d5214a93b845ce0181428ac5

출처 데이터셋

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08759384B2