Sodium Hydroxide → 1-Amino-4-bromoanthraquinone

HRID 2419233

反応式

HRID 2419233 の反応式
[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[C:5]([Br:18])=[CH:4][C:3]=1C(O)=O.[OH-].[Na+].S(S([O-])=O)([O-])=O.[Na+].[Na+]>O>[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[C:5]([Br:18])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24489Sodium DithioniteHCID 2715931-Amino-4-bromo-9,10-dioxo-9,10-dihydroanthracene-2-carboxylic acid

生成物 1

HCID 6273261-Amino-4-bromoanthraquinone収率 75%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1-Amino-4-bromoanthraquinone-2-carboxylic acid (38 grams, 0.11 mole) was dissolved in 200 ml. of water and 50 ml. of 10 M sodium hydroxide solution. The mixture was heated on a steam bath to 90°-100° C., and 40 g (b 0.23 mole) sodium hydrosulfite was added. Heating was continued with stirring for 2 hours, after which the mixture was cooled to room temperature. The resuting solid was collected by filtration and washed with water until the filtrate was neutral. The solid was dried at 80° C. to give 24.9 g (75% yield) of 1-amino-4-bromoanthraquinone. The Thin Layer Chromatogram of the crude product showed the presence of a small amount of impurity.

後処理

  1. temperatureThe mixture was heated on a steam bath to 90°-100° C.
  2. temperatureHeating
  3. filtrationThe resuting solid was collected by filtration
  4. washwashed with water until the filtrate
  5. customThe solid was dried at 80° C.

出典と根拠

ORDレコード
ord-ff9c3a58ec4e4e8ea7fef280aa9e2e86
出典データセット
uspto-grants-1978_08
特許番号
US04105680

関連ノート

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