3-(Ethoxymethylene)pentane-2,4-dione → HCID 178467925、化合物

HRID 2418949

反応式

HRID 2418949 の反応式
[CH3:1][C:2]([C:4]([C:9]([CH3:11])=[O:10])=[CH:5]OCC)=[O:3].[NH2:12][C:13]1[C:14]([Cl:24])=[C:15]([C:19]([Cl:23])=[C:20]([Cl:22])[CH:21]=1)[C:16]([OH:18])=[O:17]>C1(C)C=CC=CC=1>[CH3:11][C:9]([C:4]([C:2]([CH3:1])=[O:3])=[CH:5][NH:12][C:13]1[C:14]([Cl:24])=[C:15]([C:19]([Cl:23])=[C:20]([Cl:22])[CH:21]=1)[C:16]([OH:18])=[O:17])=[O:10]

参加物

4

反応物 2

HCID 2404183-(Ethoxymethylene)pentane-2,4-dioneHCID 198345693-Amino-2,5,6-trichlorobenzoic acid

生成物 1

HCID 178467925HCID 178467925、化合物収率 741.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
10 °C

実験手順

46.8 g (0.3 mole) of methyl 1-methylcarbonyl-2-ethoxyvinyl ketone were added dropwise to a suspension of 48.1 g (0.02 mole) of 3-amino-2,5,6-trichlorobenzoic acid in 100 ml of toluene. The mixture was heated for 2 hours to 80° C and was then cooled to 10° C, and the precipitate was filtered off. After digesting with acetonitrile, 52 g (74% of theory) of 3-[2,2-bis-(methylcarbonyl)-vinylamino]-2,5,6-trichlorobenzoic acid were obtained in the form of colourless crystals of melting point 242°-244° C.

後処理

  1. temperatureThe mixture was heated for 2 hours to 80° C
  2. filtrationthe precipitate was filtered off

出典と根拠

ORDレコード
ord-d46c7e3906b448a3880bd5b79d6480f2
出典データセット
uspto-grants-1978_08
特許番号
US04104049

関連ノート

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