Sodium Hydroxide → 1,5-Diamino-4,8-dihydroxyanthraquinone

HRID 2071314

反応式

HRID 2071314 の反応式
[N+:1]([C:4]1[C:17]2[C:16](=[O:18])[C:15]3[C:10](=[C:11]([N+:20]([O-])=O)[CH:12]=[CH:13][C:14]=3[OH:19])[C:9](=[O:23])[C:8]=2[C:7]([OH:24])=[CH:6][CH:5]=1)([O-])=O.[OH-].[Na+].[H][H]>[C].[Pd]>[NH2:1][C:4]1[C:17]2[C:16](=[O:18])[C:15]3[C:10](=[C:11]([NH2:20])[CH:12]=[CH:13][C:14]=3[OH:19])[C:9](=[O:23])[C:8]=2[C:7]([OH:24])=[CH:6][CH:5]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 30909169,10-Anthracenedione, 1,5-dihydroxy-4,8-dinitro-HCID 178418361HCID 178418361、化合物

生成物 1

HCID 673511,5-Diamino-4,8-dihydroxyanthraquinone収率 98%

試薬・触媒・溶媒 1

HCID 178418390HCID 178418390、化合物触媒

実験手順

A 500 ml. electromagnetically stirred glass reactor was charged with 5.0 g (0.0151 mole) of 1,5-dinitro-4,8-dihydroxyanthraquinone, 100 g of a 4% aqueous solution of sodium hydroxide and 0.25 g of 5% palladium-carbon. The inside of the reactor was purged with hydrogen, and the 1,5-dinitro-4,8-dihydroxyanthraquinone was hydrogenated at 50° C. with stirring. In 5 hours, 0.0906 mole of hydrogen was absorbed, whereupon the reaction was stopped. The reaction mixture was filtered to separate the catalyst. The filtrate was oxidized with air with stirring at 20° to 30° C. for 2 hours, and then neutralized with 20% sulfuric acid to a pH of 2-3. The crystals precipitated were filtered, washed with water, and dried to afford 4.0 g of 1,5-diamino-4,8-dihydroxyanthraquinone in a yield of 97.8%.

後処理

  1. customThe inside of the reactor was purged with hydrogen
  2. customwas hydrogenated at 50° C.
  3. filtrationThe reaction mixture was filtered
  4. customto separate the catalyst
  5. stirringwith stirring at 20° to 30° C. for 2 hours
  6. customThe crystals precipitated
  7. filtrationwere filtered
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-d2442c56e3b1499e9c4c1a15a419fa06
出典データセット
uspto-grants-1977_09
特許番号
US04046785

関連ノート

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