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HRID 2099710作成日:2026年10月27日

Di-tert-butyl dicarbonate → [2-(3,4-Dimethoxy-phenyl)-1-methyl-ethyl]-ethyl amine

https://huagongshe.com/reaction/2099710

反応式

関与物質

役割名称HCID仕込み量
反応物Di-tert-butyl dicarbonateHCID 90495—
反応物4-(2-(Ethylamino)propyl)-1,2-benzenediol hydrobromideHCID 130356—
反応物Sodium BicarbonateHCID 516892—
溶媒WaterHCID 962—
溶媒TetrahydrofuranHCID 8028—
生成物[2-(3,4-Dimethoxy-phenyl)-1-methyl-ethyl]-ethyl amineHCID 22061570—
生成物[2-(3,4-Dihydroxy-phenyl)-1-methyl-ethyl]-ethyl-carbamic acid tert-butyl esterHCID 70986816—

反応手順

To all of 2B from the above reaction mixture was added 30 mL of 50% THF in water. To the reaction mixture 1.1 g of sodium bicarbonate was added as a solid followed by 1.35 g (6.18 mmol) of di-t-butyl dicarbonate in 7 mL of THF dropwise over a period of 30 minutes. The reaction mixture was allowed to stir at room temperature for 18 hours, then concentrated under reduced pressure. This was diluted with 50 mL of water and the pH of the solution was adjusted to 5. The aqueous layer was extracted with 3×100 mL of ethyl acetate. The organic layers were combined, dried (anhydrous Na2SO4) and concentrated to dryness. The residue was purified by silica gel column chromatography using 30% ethyl acetate in hexane to give 764 mg (2.58 mmol, 53% from 2A) of 2C as a clear gum (M+Na, 318).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07569676B2
出典データセットuspto-grants-2009_08
ORD IDord-f2f5e5f550ac45f092d8012c30aa23a3
出典メモuspto-grants-2009_08