Hydrochloric Acid → 5-(3-Phosphonoanilino)naphthalene-2-sulfonic acid

HRID 2072329

反応式

HRID 2072329 の反応式
S(=O)(O)[O-].[Na+].[OH-].[Na+].[NH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([S:19]([OH:22])(=[O:21])=[O:20])=[CH:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=1.N[C:24]1[CH:25]=[C:26]([P:30](=[O:33])([OH:32])[OH:31])[CH:27]=[CH:28][CH:29]=1.Cl.S(=O)=O>>[P:30]([C:26]1[CH:25]=[C:24]([NH:8][C:9]2[C:18]3[C:13](=[CH:14][C:15]([S:19]([OH:22])(=[O:20])=[O:21])=[CH:16][CH:17]=3)[CH:12]=[CH:11][CH:10]=2)[CH:29]=[CH:28][CH:27]=1)([OH:33])([OH:32])=[O:31]

参加物

7

反応物 6

HCID 313Hydrochloric AcidHCID 1119Sulfur DioxideHCID 84081,6-Cleve's acidHCID 14798Sodium HydroxideHCID 79477Phosphonic acid, P-(3-aminophenyl)-HCID 23665763Sodium Bisulfite

生成物 1

HCID 214080815-(3-Phosphonoanilino)naphthalene-2-sulfonic acid

実験手順

Sodium bisulphite liquor (40% -- 23 parts), sodium hydroxide liquor (70° Tw -- 8.1 parts), salt (1.8 parts), 1-amino-6-sulphonaphtalene (11.2 parts) and 3-aminophenylphosphonic acid (10.4 parts) are heated in a sealed tube for 10 hours at 130° C. After cooling the tube is opened and hydrochloric acid (36% - 13.9 parts) is added until an acid reaction is obtained on Congo Red paper. The suspension is boiled under reflux for 1 hour until evolution of sulphur dioxide has essentially ceased. During this period samples are spotted on to Congo Red paper to confirm acid reaction. The suspension is cooled to room temperature and filtered. The filtrate is set stirring and sodium chloride (8 parts = 20% wt/vol) added. After stirring for 18 hours the suspension is filtered under vacuum and the cake pressed well to remove mothers liquor. The paste (8 parts) is dried in air at 50°-60° C to give 7 parts of 1-(3-phosphonophenylamino)-6-sulphonaphthalene.

後処理

  1. temperatureAfter cooling the tube
  2. customis obtained on Congo Red paper
  3. customreaction
  4. filtrationfiltered
  5. additionsodium chloride (8 parts = 20% wt/vol) added
  6. stirringAfter stirring for 18 hours the suspension
  7. filtrationis filtered under vacuum
  8. customto remove mothers liquor
  9. customThe paste (8 parts) is dried in air at 50°-60° C

出典と根拠

ORDレコード
ord-2d05a617a8a2480e83c823609123cfe6
出典データセット
uspto-grants-1977_09
特許番号
US04051175

関連ノート

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