戻る
化工社化工社 化学情報印刷レポート · 研究参考用
HRID 1040587作成日:2026年10月26日

Dichloromethane methanol → 2-[5-Chloro-2-(1-oxo-2,3,4,5-tetrahydro-1H-benzo[c]azepin-7-ylamino)-pyrimidin-4-ylamino]-N-methyl-benzamide

https://huagongshe.com/reaction/1040587

反応式

関与物質

役割名称HCID仕込み量
反応物Dichloromethane methanolHCID 21226129—
反応物2-(2,5-Dichloropyrimidin-4-ylamino)-N-methylbenzamideHCID 57974132—
反応物7-amino-2,3,4,5-tetrahydro-1H-benzo[c]azepin-1-oneHCID 59862347—
溶媒2-MethoxyethanolHCID 8019—
生成物2-[5-Chloro-2-(1-oxo-2,3,4,5-tetrahydro-1H-benzo[c]azepin-7-ylamino)-pyrimidin-4-ylamino]-N-methyl-benzamideHCID 2515702725%

反応条件

温度120 °C

反応手順

7-Amino-2,3,4,5-tetrahydro-benzo[c]azepin-1-one (21 mg, 0.12 mmol) and 2-(2,5-dichloro-pyrimidin-4-ylamino)-N-methyl-benzamide (36 mg, 0.12 mmol) were suspended in 2-methoxyethanol (1 ml), and heated to 120° C. for 5 hours. Concentration afforded a yellow solid. Preparative TLC (5% MeOH/CH2Cl2) gave the title compound the desired as a white solid, 13 mg. (25% yield) 1H NMR (400 MHz, DMSO-d6) δ 11.59 (s, 1H), 9.68 (s, 1H), 8.68-8.77 (m, 2H), 8.30 (s, 1H), 7.80-7.86 (m, 1H), 7.71-7.78 (m, 1H), 7.59 (s, 2H), 7.43-7.51 (m, 1H), 7.34-7.39 (m, 1H), 7.12-7.18 (m, 1H), 2.85-2.97 (m, 2H), 2.79 (s, 3H), 2.60-2.71 (m, 2H), 1.80-1.90 (m, 2H); MS (m/e) 437 (M+1).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08552186B2
出典データセットuspto-grants-2013_10
ORD IDord-4841561d3f284f49b30fc3ff6704bdad
出典メモuspto-grants-2013_10