Formaldehyde → 1-Amino-2-bromo-4-hydroxyanthraquinone

HRID 1905848

反応式

HRID 1905848 の反応式
OS(O)(=O)=O.O=S(=O)=O.C=[O:11].[NH2:12][C:13]1[C:26]2[C:25](=[O:27])[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[C:18](=[O:28])[C:17]=2[C:16](Br)=[CH:15][C:14]=1[Br:30]>O>[NH2:12][C:13]1[C:26]2[C:25](=[O:27])[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[C:18](=[O:28])[C:17]=2[C:16]([OH:11])=[CH:15][C:14]=1[Br:30]

参加物

5

反応物 3

HCID 712FormaldehydeHCID 66811-Amino-2,4-dibromoanthraquinoneHCID 24681Fuming sulfuric acid

生成物 1

HCID 83201-Amino-2-bromo-4-hydroxyanthraquinone収率 93.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

Hydrolysis is carried out by adding 195.3 parts of 66% oleum and 16 parts of paraformaldehyde to the reaction mixture and heating it to 110° C. The mixture is heated in a stream of nitrogen to 110° C. until the presence of 1-amino-2,4-dibromoanthraquinone can no longer be detected. The reaction time is from 1 to 2 hours. Upon completion of the reaction, the reaction mixture is cooled to room temperature and diluted with 523 parts of water. The precipitated crystals of 1-amino-2-bromo-4-hydroxyanthraquinone are isolated by filtration and washed with water until neutral, affording 149 parts of product, corresponding to a yield of 93.7%, based on 1-aminoanthraquinone. Melting point: 226°-228° C. (lit.: 231°-232° C.). According to elemental analysis, the bromine content is 25.0% (calculated: 25.2%).

後処理

  1. customHydrolysis
  2. customUpon completion of the reaction
  3. temperaturethe reaction mixture is cooled to room temperature

出典と根拠

ORDレコード
ord-a6ea770377d74cb7b3b2f253466d2d71
出典データセット
uspto-grants-1987_03
特許番号
US04648994

関連ノート

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