Sulfuric Acid → HCID 67884339、化合物

HRID 257475ノート

反応式

HRID 257475 の反応式
[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

参加物

6

反応物 3

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 19783310HCID 19783310、化合物

生成物 2

HCID 19783363HCID 19783363、化合物収率 11.5%HCID 67884339HCID 67884339、化合物収率 33.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-25d3738c78eb4924a4fa67351b6c44af
出典データセット
uspto-grants-1993_11
特許番号
US05262420

反応ノート

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