Hydrochloric Acid → 1-Amino-4-(5'-amino-2'-methylphenylamino)-anthraquinone-2-sulphonic acid

HRID 568317ノート

反応式

HRID 568317 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)=[CH:4][C:3]=1[S:19]([OH:22])(=[O:21])=[O:20].C(=O)([O-])[O-].[Na+].[Na+].C([NH:32][C:33]1[CH:38]=[CH:37][C:36]([CH3:39])=[C:35]([NH2:40])[CH:34]=1)(=O)C.Cl>O.C(O)(C)C>[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]([NH:40][C:35]2[CH:34]=[C:33]([NH2:32])[CH:38]=[CH:37][C:36]=2[CH3:39])=[CH:4][C:3]=1[S:19]([OH:22])(=[O:21])=[O:20]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 10340Sodium Carbonate2 回HCID 226281-Amino-4-bromo-9,10-dihydro-9,10-dioxo-2-anthracenesulfonic acidHCID 22865N-(3-amino-4-methylphenyl)acetamide

生成物 1

HCID 201500481-Amino-4-(5'-amino-2'-methylphenylamino)-anthraquinone-2-sulphonic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3776Isopropanol溶媒

反応条件

温度
80 °C

実験手順

38.2 Parts 1-amino-4-bromoanthraquinone-2-sulphonic acid are dissolved in 200 parts water/100 parts i-propanol and the pH adjusted to 8.5-9.0 with sodium carbonate. After addition of 18 parts 4-acetylamino-2-aminotoluene the mixture is warmed to 80° C. and treated with 1 part cuprous chloride and 12 parts sodium carbonate. After 4 hours the reaction is over. Finally 25 parts 30% hydrochloric acid are added to the reaction mixture, which is then heated to reflux. After 18 hours the suspension is cooled to room temperature, filtered and washed with 1% hydrochloric acid, to give 1-amino-4-(5'-amino-2'-methylphenylamino)-anthraquinone-2-sulphonic acid.

後処理

  1. temperatureis then heated to reflux
  2. temperatureAfter 18 hours the suspension is cooled to room temperature
  3. filtrationfiltered
  4. washwashed with 1% hydrochloric acid

出典と根拠

ORDレコード
ord-f7fe5edc58404c08adc817af9b395f9c
出典データセット
uspto-grants-1988_03
特許番号
US04728464

反応ノート

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