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HRID 234751作成日:2026年10月24日

2-Chlorophenol → 2,5-Cyclohexadien-1-one, 2-chloro-4-((4-(diethylamino)-2-methylphenyl)imino)-

https://huagongshe.com/ja/reaction/234751

反応式

関与物質

役割名称HCID仕込み量
反応物2-ChlorophenolHCID 7245—
反応物Sodium CarbonateHCID 10340—
反応物N,N-Diethyltoluene-2,5-diamine hydrochlorideHCID 108623—
溶媒EthanolHCID 702—
溶媒MethanolHCID 887—
溶媒WaterHCID 962—
生成物2,5-Cyclohexadien-1-one, 2-chloro-4-((4-(diethylamino)-2-methylphenyl)imino)-HCID 10967590%

反応条件

温度55 °C

反応手順

1450 parts K3Fe(CN)6, 595 parts Na2CO3, and 4150 parts water were added to a 12-liter round bottom flask equipped with a mechanical stirrer, thermometer, and addition funnel. The mixture was heated to 55° C. with stirring. A solution of 227 parts 4-(N,N-diethylamino)-2-methylaniline monohydrochloride, 128 parts o-chlorophenol, 1960 parts ethanol, and 2500 parts water was charged to the addition funnel and added dropwise to the stirred, heated solution. After the addition was complete the reaction mixture was maintained at 55° C. with stirring for 20 minutes. The warm mixture was filtered with vacuum and the resulting filter cake was placed in a solution of 296 parts ethanol and 1125 parts water to form a slurry. The dye was isolated by vacuum filtration. This process was repeated two times, first with 296 parts ethanol and 1125 parts water, then with 608 parts methanol. After the final vacuum filtration the filter cake was dried at 40° C. under vacuum for 48 hours. Yield was ~90%. The final product can be recrystallized from ethyl acetate or ethanol.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05596025
出典データセットuspto-grants-1997_01
ORD IDord-084edde874f649ec9ddd0f2e85d1e229
出典メモuspto-grants-1997_01