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HRID 636474作成日:2026年10月25日

Hydrazine hydrate (1:1) → 3-(Tert-butyldiphenylsilyloxymethyl)-2,4-dichloroaniline

https://huagongshe.com/reaction/636474

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrazine hydrate (1:1)HCID 24654—
反応物1-(Tert-butyldiphenylsilyloxymethyl)-2,6-dichloro-3-nitrobenzeneHCID 11798185—
溶媒MethanolHCID 887—
溶媒WaterHCID 962—
生成物3-(Tert-butyldiphenylsilyloxymethyl)-2,4-dichloroanilineHCID 1059871986%

反応手順

To a stirred mixture of 1-(tert-butyldiphenylsilyloxy-methyl)-2,6-dichloro-3-nitrobenzene (433 mg), ferric chloride hexahydrate (17.5 mg) and activated carbon (17.5 mg) in a mixture of methanol (2.78 ml) and water (0.69 ml) was added hydrazine monohydrate (0.135 ml) dropwise at 60-70° C. After the addition was finished, the mixture was refluxed for half an hour. The mixture was allowed to cool and filtered. The filtrate was concentrated in vacuo. The residue was extracted with dichloromethane and the organic phase was dried over anhydrous magnesium sulfate. After being filtered, the filtlate was concentrated in vacuo and the resulting residue was washed with n-hexane to give 3-amino-1-(tert-butyldiphenylsilyloxymethyl)-2,6-dichlorobenzene (348 mg) as a white mass.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06194396B1
出典データセットuspto-grants-2001_02
ORD IDord-0cf490bdb91e4ca68f1362a6224b60c5
出典メモuspto-grants-2001_02