P-Anisidine → 1-p-Anisidino-8-nitro-anthraquinone

HRID 2418996

反応式

HRID 2418996 の反応式
[N+:1]([C:4]1[C:17]2[C:16](=[O:18])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][C:14]=3[N+:19]([O-:21])=[O:20])[C:9](=[O:22])[C:8]=2[CH:7]=[CH:6][CH:5]=1)([O-])=O.[CH3:23][O:24][C:25]1[CH:30]=[CH:29][C:28](N)=[CH:27][CH:26]=1.C([O-])(=O)C.[K+]>CO>[CH3:23][O:24][C:25]1[CH:30]=[CH:29][C:28]([NH:1][C:4]2[C:17]3[C:16](=[O:18])[C:15]4[C:10](=[CH:11][CH:12]=[CH:13][C:14]=4[N+:19]([O-:21])=[O:20])[C:9](=[O:22])[C:8]=3[CH:7]=[CH:6][CH:5]=2)=[CH:27][CH:26]=1

参加物

5

反応物 3

HCID 7732P-AnisidineHCID 672101,8-Dinitro-9,10-anthraquinoneHCID 517044Potassium Acetate

生成物 1

HCID 203164861-p-Anisidino-8-nitro-anthraquinone

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 50 g. of 1,8-dinitro-anthraquinone (82% strength), 150 g of p-anisidine and 21.5 g of anhydrous potassium acetate is heated at 95° - 100° C (duration approx. 5 hours), with vigorous stirring, until no further starting material is present, according to thin layer chromatography. The mixture is diluted with 150 ml of methanol over the course of 30 minutes at 50° - 60° C and is stirred overnight until cold and the reaction product is filtered off, washed with a solution of 30 g of p-anisidine in 30 ml of methanol and finally with 200 ml of methanol and hot water, and dried at 80° C. 51 g of 1-p-anisidino-8-nitro-anthraquinone are obtained.

後処理

  1. additionA mixture of 50 g
  2. filtrationis filtered off
  3. washwashed with a solution of 30 g of p-anisidine in 30 ml of methanol and finally with 200 ml of methanol and hot water
  4. customdried at 80° C

出典と根拠

ORDレコード
ord-70d7d2e2fed24dc581be857afa5daee4
出典データセット
uspto-grants-1978_08
特許番号
US04104284

関連ノート

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