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HRID 1673443作成日:2026年10月26日

2,3-Dimethylbenzoic acid → Tert-butyl 4-(benzo[1,3]dioxol-5-yl)-2-(2,3-dimethylbenzamido)benzoate

https://huagongshe.com/reaction/1673443

反応式

関与物質

役割名称HCID仕込み量
反応物2,3-Dimethylbenzoic acidHCID 11782—
反応物Oxalyl chlorideHCID 65578—
反応物Sodium BicarbonateHCID 516892—
反応物Tert-butyl 2-amino-4-(benzo[1,3]dioxol-5-yl)benzoateHCID 67342168—
溶媒DimethylformamideHCID 6228—
溶媒DichloromethaneHCID 6344—
溶媒TriethylamineHCID 8471—
生成物Tert-butyl 4-(benzo[1,3]dioxol-5-yl)-2-(2,3-dimethylbenzamido)benzoateHCID 67342913—

反応手順

1.7 mL of methylene chloride, 1.0 μL N,N-dimethylformamide and 0.025 mL of oxalyl chloride were added to 41 mg of 2,3-dimethylbenzoic acid at room temperature sequentially and stirred ad the same temperature for 1 hour. The reaction mixture was added to a mixed solution of 50 mg of tert-butyl 2-amino-4-(benzo[1,3]dioxol-5-yl)benzoate, 2.8 mL of methylene chloride and 0.36 mL of triethylamine and stirred at room temperature for 1 hour. A saturated sodium hydrogen carbonate aqueous solution was added to the reaction mixture, and the organic layer was separated, and the solvent was evaporated under reduced pressure. The obtained residue was purified with silica gel column chromatography [Flash Tube 2008 manufactured by Trikonex Company, eluent; hexane:ethyl acetate=4:1]to obtain tert-butyl 4-(benzo[1,3]dioxol-5-yl)-2-(2,3-dimethylbenzamido)benzoate.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07999132B2
出典データセットuspto-grants-2011_08
ORD IDord-34f7e69ca54144a6b2fbb6e009767c56
出典メモuspto-grants-2011_08