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HRID 853697作成日:2026年10月26日

Hydrochloric Acid → HCID 178490840、化合物

https://huagongshe.com/reaction/853697

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物Sodium hydrideHCID 24758—
反応物2,3-Dimethyl 2,3-pyridinedicarboxylateHCID 69058—
反応物1-(2,4-Dimethoxybenzyl)pyrrolidine-2,5-dioneHCID 11391014—
溶媒MethanolHCID 887—
溶媒Diethyl EtherHCID 3283—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 178490840HCID 17849084052%

反応条件

温度80 °C

反応手順

To 1-(2,4-dimethoxy-benzyl)-pyrrolidine-2,5-dione 299 (1.4 g, 5.6 mmol) and pyridine-2,3-dicarboxylic acid dimethyl ester (1.13 g, 5.8 mmol) dissolved in tetrahydrofuran (60 ml) and methanol (7.0 ml) was added a 60% dispersion of sodium hydride in mineral oil (NaH, 492 mg, 12.3 mmol). The reaction mixture was warmed to 80° C. and kept at 80° C. with stirring overnight. The reaction mixture was placed in an ice bath and titrated to a pH of 4 with 1 M HCl. 200 ml of ether was added and the resulting yellow solid was collected by filtration. The solid was washed twice with ether, twice with water, and dried under high vacuum with heating to provide 7-(2,4-dimethoxy-benzyl)-5,9-dihydroxy-pyrrolo[3,4-g]quinoline-6,8-dione 300 (1.1 g, 52%). 1H NMR (d-DMSO) δ 10.8 (broad, 2H), 9.0 (d, 1H), 8.67 (d, 1H), 7.72 (m, 1H), 6.90 (d, 1H), 6.5 (d, 1H), 6.38 (dd, 1H), 4.58 (s, 2H), 3.76 (s, 3H), 3.66 (s, 3H). MS: 382.1 (M+1)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07253180B2
出典データセットuspto-grants-2007_08
ORD IDord-7adba5056dd74c53b5a131f5b6310119
出典メモuspto-grants-2007_08