Phosphorus oxychloride → HCID 178490023、化合物

関与物質

役割	名称	HCID	仕込み量
反応物	Phosphorus oxychloride	HCID 24813	—
反応物	3-(3,4-Dimethoxyphenyl)propionyl chloride	HCID 15620702	—
反応物	1H-benzimidazole-5-carbohydrazide	HCID 16637119	—
生成物	HCID 178490023	HCID 178490023	—

反応手順

The compound was synthesized starting from benzimidazol-5-carbohydrazide (176 mg, 1 mmol), TEA (0.153 ml; 1.1 mmol), 3,4-dimethoxyphenylpropionylchloride (228 mg, 1.1 mmol) and POCl3 (0.5 ml; 5.5 mmol) as described in method 1; yield: 0.019 mg (5.4%); MS m/z: 351.3 [M+H]+; 1H-NMR (DMSO d6, 400 MHz): δ 3.04 (t, 2H, 3J=7.5 Hz); 3.23 (t, 2H, 3J=7.5 Hz); 3.69 (s, 6H); 6.78 (dd, 1H, 4J=1.7 Hz, 3J=8.3 Hz); 6.84 (d, 1H, 3J=8.3 Hz); 6.90 (d, 1H, 4J=1.7 Hz); 7.76 (d, 1H, 3J=8.3 Hz); 7.83 (dd, 1H, 4J=1.7 Hz, 3J=8.3 Hz); 8.17 (br s, 1H), 8.40 (s, 1H); HPLC (METHOD [A]): rt 10.29 min (94.2%)

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US09181233B2
出典データセット	uspto-grants-2015_11
ORD ID	ord-701367b8aa064b6cacf68600e54b6556
出典メモ	uspto-grants-2015_11