Sodium Hydroxide → 1-Amino-4-bromoanthraquinone

HRID 2419233

반응식

HRID 2419233 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 6273261-Amino-4-bromoanthraquinone수율 75%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-ff9c3a58ec4e4e8ea7fef280aa9e2e86
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04105680

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