Sulfuric Acid → HCID 67884339, 화합물

HRID 257475노트

반응식

HRID 257475 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7](O)([CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH3:8])=[CH:3][CH:2]=1.S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>O>[C:11]1([CH2:10]/[CH:9]=[C:7](/[C:4]2[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=2)\[CH3:8])[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1.[C:11]1([CH2:10][CH2:9][C:7]([C:4]2[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=2)=[CH2:8])[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 19783310HCID 19783310, 화합물

생성물 2

HCID 19783363HCID 19783363, 화합물수율 11.5%HCID 67884339HCID 67884339, 화합물수율 33.7%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

To the said alcoholic substance, that is 1.42 g of 2-(4-pyridyl)-4-phenyl-2-butanol, 4 ml of 65% sulfuric acid was added and the mixture was stirred for two hours at 100° C. After cooling, water was added and the mixture was alkalized with sodium carbonate to extract with ethyl acetate. After drying over anhydrous sodium sulfate, the solvent was distilled away under reduced pressure to obtain viscous oily substance. The said oily substance was purified by silica gel column chromatography to obtain 0.44 g of (E)-1-phenyl-3-(4-pyridyl)-2-butene (yield: 33.7%) and 0.15 g of 4-phenyl-2-(4-pyridyl)-1-butene (yield: 11.5%).

후처리

  1. additionwas added
  2. temperatureAfter cooling
  3. extractionto extract with ethyl acetate
  4. dry with materialAfter drying over anhydrous sodium sulfate
  5. distillationthe solvent was distilled away under reduced pressure
  6. customto obtain viscous oily substance
  7. customThe said oily substance was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-25d3738c78eb4924a4fa67351b6c44af
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05262420

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