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HRID 1881627作成日:2026年10月25日

p-Toluenesulfonic acid monohydrate → Methyl 4-[(2-{1-[2-bromo-5-(4-t-butylphenyl)-4-hydroxy-3-thienyl]ethylidene}hydrazino)carbonyl]benzoate

https://huagongshe.com/reaction/1881627

反応式

関与物質

役割名称HCID仕込み量
反応物p-Toluenesulfonic acid monohydrateHCID 521998—
反応物Chloroform ethylacetateHCID 21584013—
反応物2-Bromo-5-(4-t-butylphenyl)-4-hydroxy-3-methylcarbonylthiopheneHCID 67050460—
反応物4-HydrazinocarbonylmethylbenzoateHCID 131727585—
溶媒IsopropanolHCID 3776—
生成物Methyl 4-[(2-{1-[2-bromo-5-(4-t-butylphenyl)-4-hydroxy-3-thienyl]ethylidene}hydrazino)carbonyl]benzoateHCID 7236000562%

反応手順

To a suspension of 2-bromo-5-(4-t-butylphenyl)-4-hydroxy-3-methylcarbonylthiophene (1.00 g, 2.83 mmol) synthesized in Reference Synthetic Example 55 and 4-hydrazinocarbonylmethylbenzoate (550 mg, 2.83 mmol) in isopropyl alcohol (28.3 mL), tosylic acid monohydrate (146 mg, 0.85 mmol) was added, and the mixture was heated with reflux for about 1 hour. The reaction solution was concentrated, and then purified with a silica gel column chromatography (chloroform, and then chloroform/ethyl acetate=95/5) to obtain the desired product as a yellow solid (935 mg, yield 62%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08318796B2
出典データセットuspto-grants-2012_11
ORD IDord-6c2c5877abe346b58f80024c4d01bc89
出典メモuspto-grants-2012_11