Iodine → HCID 20470550, 화합물

HRID 1388243노트

반응식

HRID 1388243 반응식
[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

참가 물질

9

반응물 5

HCID 807Iodine2회HCID 1118Sulfuric AcidHCID 24345Iodic acidHCID 24477Sodium ThiosulfateHCID 204705634-(2-Methoxyethyl)-1,1'-biphenyl

생성물 1

HCID 20470550HCID 20470550, 화합물수율 231%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매HCID 5943Carbon Tetrachloride용매

반응 조건

온도
83 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-dca8434e973242e29f4406eec8532ad8
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04431564

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