Ethylene Glycol → HCID 59660700, 화합물

HRID 1641430노트

반응식

HRID 1641430 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13]([CH3:14])=[C:12]([CH:15]=[O:16])[CH:11]=[N:10]2)=[CH:5][CH:4]=1.[CH2:17](O)[CH2:18][OH:19].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[O:16]1[CH2:17][CH2:18][O:19][CH:15]1[C:12]1[CH:11]=[N:10][N:9]([C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=2)[C:13]=1[CH3:14]

참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 27797351-(4-Methoxyphenyl)-5-methyl-1H-pyrazole-4-carbaldehyde

생성물 1

HCID 59660700HCID 59660700, 화합물수율 58.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 1-(4-methoxy-phenyl)-5-methyl-1H-pyrazole-4-carbaldehyde (0.5 g, 2.3 mmol), ethylene glycol (1.44 g, 23.1 mmol) and p-toluenesulfonic acid (0.2 g, 1.2 mmol) in toluene (10 mL) was refluxed for 18 h (Dean Stock to remove water formed). After it was allowed to cool to room temperature, the reaction mixture was diluted with ethyl acetate, washed with sat. NaHCO3 (aq) and brine, and dried over Na2SO4. After concentrated, the residue was purified by a column chromatography on silica gel to yield the title compound (0.35 g, 58%); MS (APCI) m/z: 261 (M+1, 80).

후처리

  1. temperaturewas refluxed for 18 h
  2. custom(Dean Stock to remove water formed)
  3. additionthe reaction mixture was diluted with ethyl acetate
  4. washwashed with sat. NaHCO3 (aq) and brine
  5. dry with materialdried over Na2SO4
  6. concentrationAfter concentrated
  7. customthe residue was purified by a column chromatography on silica gel

출처 및 근거

ORD 기록
ord-a6db0c52a4614a47882bc7d6906dede7
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08115005B2

반응 노트

불러오는 중…