Iodine → HCID 20470550、化合物

HRID 1388243ノート

反応式

HRID 1388243 の反応式
[CH3:1][O:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:7][CH:6]=1.[I:17](O)(=O)=O.II.S(=O)(=O)(O)O.S([O-])([O-])(=O)=S.[Na+].[Na+]>C(Cl)(Cl)(Cl)Cl.O.C(O)(=O)C>[CH3:1][O:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([I:17])=[CH:13][CH:12]=2)=[CH:7][CH:6]=1

参加物

9

反応物 5

HCID 807Iodine2 回HCID 1118Sulfuric AcidHCID 24345Iodic acidHCID 24477Sodium ThiosulfateHCID 204705634-(2-Methoxyethyl)-1,1'-biphenyl

生成物 1

HCID 20470550HCID 20470550、化合物収率 231%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 5943Carbon Tetrachloride溶媒

反応条件

温度
83 °C

実験手順

Into a 300 ml three-neck flask were added 4-(β-methyloxyethyl) biphenyl (34 g, 0.16 mol), acetic acid (112 ml), water (30 ml), iodic acid (6.8 g, 0.0384 mol), iodine (17.9 g, 0.0704 mol), carbon tetrachloride (13 ml) and conc. sulfuric acid (4.8 ml). The mixture was warmed by a mantle heater with stirring, and reaction was carried out under reflux at 83° C. for 3 hours. After completion of the reaction, the reaction liquid was cooled down to 70° C., and 10% sodium thiosulfate aqueous solution (10 ml) was added to cause excess iodine to disappear. The liquid was cooled down to room temperature, and the precipitated crystals were recrystallized from ethyl ethanol (300 ml) to obtain 4'-(β-methoxyethyl)-4-iodobiphenyl (V) (30 g) having a melting point of 97°~99.4° C.

後処理

  1. temperatureThe mixture was warmed by a mantle heater
  2. customreaction
  3. customAfter completion of the reaction
  4. customthe reaction liquid
  5. temperaturewas cooled down to 70° C.
  6. temperatureThe liquid was cooled down to room temperature
  7. customthe precipitated crystals were recrystallized from ethyl ethanol (300 ml)

出典と根拠

ORDレコード
ord-dca8434e973242e29f4406eec8532ad8
出典データセット
uspto-grants-1984_02
特許番号
US04431564

反応ノート

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