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HRID 372831作成日:2026年10月26日

Acetic Acid → 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodo-1'-methylspiro[2H-1,3-benzoxazin-2,4'-piperidine]

https://huagongshe.com/reaction/372831

反応式

関与物質

役割名称HCID仕込み量
反応物Acetic AcidHCID 176—
反応物1-Methyl-4-piperidoneHCID 74049—
反応物2-Aminomethyl-4-t-butyl-6-iodophenolHCID 119286—
溶媒BenzeneHCID 241—
生成物3,4-dihydro-6-(1,1-dimethylethyl)-8-iodo-1'-methylspiro[2H-1,3-benzoxazin-2,4'-piperidine]HCID 1285790057.5%

反応手順

A mixture of 2-aminomethyl-4-(1,1-dimethylethyl)-6-iodophenol (6.0 g., 0.02 mole), 1-methyl-4-piperidone (2.24 g., 0.02 mole), acetic acid (2 ml.) and benzene (100 ml.) is refluxed under a Dean-Stark trap for 4 hrs. The clear yellow solution then is washed with 2% sodium hydroxide solution, water and salt brine and dried (MgSO4). The residue that remains after evaporation of the benzene is crystallized from ethanol to obtain 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodo-1'-methylspiro[2H-1,3-benzoxazin-2,4'-piperidine], (4.6 g.), m.p. 155°-156.5° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04092414
出典データセットuspto-grants-1978_05
ORD IDord-d7b212be02cb4b459c195496c9ce6734
出典メモuspto-grants-1978_05