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Sulfuric Acid → HCID 54345768、化合物

HRID 1438844
ノート
印刷プレビュー

反応式

HRID 1438844 の反応式
S(=O)(=O)(O)O.[CH2:6]([O:8][C:9](=[O:19])[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([NH2:17])[C:11]=1[Cl:18])[CH3:7].O[CH2:21][S:22]([C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=1)(=[O:24])=[O:23]>O>[CH2:6]([O:8][C:9](=[O:19])[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([NH:17][CH2:21][S:22]([C:25]2[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=2)(=[O:24])=[O:23])[C:11]=1[Cl:18])[CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 18994119Ethyl 3-amino-2,5-dichlorobenzoateHCID 19820153HCID 19820153、化合物

生成物 1

HCID 54345768HCID 54345768、化合物収率 71%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1 g of concentrated sulfuric acid was added to 2.32 g (10mmoles) of 2,5-dichloro-3-aminobenzoic acid ethyl ester, 2.27 g (11mmoles) of hydroxymethyl-(4-chlorophenyl)-sulfone and 40 ml of water whilst stirring at room temperature. The mixture was stirred for a further 3 hours at room temperature, the solid was filtered off and dissolved in about 100 ml of methylene chloride, the solution was dried over magnesium sulfate and worked up in the usual manner and the product was recrystallized from ethylene chloride. 3.0 g (71% of theory) of 2,5-dichloro-3-[(4-chlorophenyl)-sulfonylmethylamino]-benzoic acid ethyl ester were obtained in the form of colorless crystals of melting point 173°-175° C.

後処理

  1. stirringThe mixture was stirred for a further 3 hours at room temperature
  2. filtrationthe solid was filtered off
  3. dissolutiondissolved in about 100 ml of methylene chloride
  4. dry with materialthe solution was dried over magnesium sulfate
  5. customthe product was recrystallized from ethylene chloride

出典と根拠

ORDレコード
ord-940a81a65d644590b07f98b76862b519
出典データセット
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04057418

反応ノート

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