Hydrochloric Acid → HCID 10978507, 화합물

HRID 1419733노트

반응식

HRID 1419733 반응식
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

참가 물질

4

반응물 3

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

생성물 1

HCID 10978507HCID 10978507, 화합물수율 96%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-fc53bf48f1df43e9aa8a6051855c7a4c
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05889002

반응 노트

불러오는 중…