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Sulfuric Acid → HCID 21506021、化合物

HRID 918687
ノート
印刷プレビュー

反応式

HRID 918687 の反応式
NC1C=C(C=C(S(=O)(=O)N)C=1NC1C=CC=CC=1)C(O)=O.OS(O)(=O)=O.[NH:27]([C:34]1[C:46]([S:47](=[O:50])(=[O:49])[NH2:48])=[CH:45][C:37]([C:38]([O:40]CCCC)=[O:39])=[CH:36][C:35]=1[NH:51][CH2:52][CH2:53][CH2:54][CH3:55])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[OH-].[Na+]>O.C(O)CCC>[NH:27]([C:34]1[C:46]([S:47](=[O:50])(=[O:49])[NH2:48])=[CH:45][C:37]([C:38]([OH:40])=[O:39])=[CH:36][C:35]=1[NH:51][CH2:52][CH2:53][CH2:54][CH3:55])[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 21505992HCID 21505992、化合物HCID 21506098HCID 21506098、化合物

生成物 1

HCID 21506021HCID 21506021、化合物

試薬・触媒・溶媒 2

HCID 2631-Butanol溶媒
HCID 962
Water
溶媒

実験手順

A mixture of 3-amino-4-anilino-5-sulphamyl-benzoic acid (4 g), n-butanol (50 ml), and conc. H2SO4 (0.4 ml) was boiled under reflux with water separator for 5 days. The resulting solution of butyl 4-anilino-3-butylamino-5-sulphamyl-benzoate was saponified by addition of 2N sodium hydroxide and boiling under reflux for 45 minutes. After neutralization with 4N hydrochloric acid, the reaction mixture was evaporated in vacuo. The residue was dissolved in hot water (50 ml), and the 4-anilino-3-butylamino-5-sulphamyl-benzoic acid was precipitated by addition of 4N hydrochloric acid to pH 3. The crude acid was dissolved in diethyl ether (50 ml), and undissolved impurities were filtered off. The etherial solution was evaporated to dryness, and the residue was recrystallized from acetone-water and aqueous ethanol, after which the compound was obtained with a melting point of 230-231°C.

後処理

  1. temperatureunder reflux for 45 minutes
  2. customAfter neutralization with 4N hydrochloric acid, the reaction mixture was evaporated in vacuo
  3. dissolutionThe residue was dissolved in hot water (50 ml)
  4. customthe 4-anilino-3-butylamino-5-sulphamyl-benzoic acid was precipitated by addition of 4N hydrochloric acid to pH 3
  5. dissolutionThe crude acid was dissolved in diethyl ether (50 ml)
  6. filtrationundissolved impurities were filtered off
  7. customThe etherial solution was evaporated to dryness
  8. customthe residue was recrystallized from acetone-water and aqueous ethanol
  9. customafter which the compound was obtained with a melting point of 230-231°C.

出典と根拠

ORDレコード
ord-5c28b90ea50a4b2baaa687c4b56dead6
出典データセット
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03971819

反応ノート

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