Ethanol → HCID 15408136, 화합물

HRID 1275699노트

반응식

HRID 1275699 반응식
[CH2:1]([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([C:17]2[O:18][C:19]([C:22]([OH:24])=[O:23])=[CH:20][CH:21]=2)=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[K].[CH2:26](O)[CH3:27].S(=O)(=O)(O)O>C1(C)C=CC=CC=1.O>[CH2:1]([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([C:17]2[O:18][C:19]([C:22]([O:24][CH2:26][CH3:27])=[O:23])=[CH:20][CH:21]=2)=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 5462222PotassiumHCID 10925187HCID 10925187, 화합물

생성물 1

HCID 15408136HCID 15408136, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

52.4 g (0.15 mol) of 1-benzyl-3-(5-carboxy-2-furyl)indazole, potassium salt, were initially charged in 1250 ml of toluene, and after addition of 200 ml of abs. ethanol and 50 ml of conc. sulfuric acid the mixture was stirred under reflux on a water separator. After 3 hours, the mixture was concentrated using a rotary evaporator, the oil that remained was taken up in water/ethyl acetate and the aqueous phase was separated off. The organic phase was washed with water and 7.5% strength NaHCO3 solution, dried with sodium sulfate and concentrated. The residue was recrystallized from isopropanol. This gave 37.8 g (73%) of the title compound. m.p.: 98-99 ° C.

후처리

  1. additionafter addition of 200 ml of abs
  2. concentrationthe mixture was concentrated
  3. customa rotary evaporator
  4. customthe aqueous phase was separated off
  5. washThe organic phase was washed with water and 7.5% strength NaHCO3 solution
  6. dry with materialdried with sodium sulfate
  7. concentrationconcentrated
  8. customThe residue was recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-6310154fd1ab4dbb9278a5366a4663e6
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06162819

반응 노트

불러오는 중…