Hydrochloric Acid → HCID 10978507、化合物

HRID 1419733ノート

反応式

HRID 1419733 の反応式
C([NH:5][S:6]([C:9]1[S:10][C:11]([Cl:17])=[CH:12][C:13]=1[C:14]([OH:16])=[O:15])(=[O:8])=[O:7])(C)(C)C.Cl.[CH2:19](O)[CH3:20]>>[Cl:17][C:11]1[S:10][C:9]([S:6](=[O:7])(=[O:8])[NH2:5])=[C:13]([C:14]([O:16][CH2:19][CH3:20])=[O:15])[CH:12]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 104473715-Chloro-2-[[(1,1-dimethylethyl)amino]sulfonyl]-3-thiophenecarboxylic acid

生成物 1

HCID 10978507HCID 10978507、化合物収率 96%

実験手順

A solution of 2-(N-tert-butylsulfamoyl)-5-chlorothiophene-3-carboxylic acid (60.0 g; 0.201 mol) made by the procedure described by B. Unterhalt and S. Moghaddam, Pharmazie 49, 115-117 (1994) in 700 ml of abs. ethanol saturated with hydrogen chloride was heated with stirring at reflux for 17 h. The cooled solution was evaporated to dryness and the residue was purified by trituration with water and dried to give 52.3 g (96%) of the title compound; 1H-NMR (DMSO-d6): δ 1.31 (t, J=7 Hz, 3H, CH3), 4.32 (q, J=7 Hz, 2H, CH2), 7.55 (s, 1H), 7.77 (br. s, 2H, NH2).

後処理

  1. temperatureat reflux for 17 h
  2. customThe cooled solution was evaporated to dryness
  3. customthe residue was purified by trituration with water
  4. customdried

出典と根拠

ORDレコード
ord-fc53bf48f1df43e9aa8a6051855c7a4c
出典データセット
uspto-grants-1999_03
特許番号
US05889002

反応ノート

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