Hydrochloric Acid → 4-Hydroxy-3-iodobiphenyl

HRID 1432048

반응식

HRID 1432048 반응식
[C:1]1([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][C:4]([OH:7])=[CH:3][CH:2]=1.[I-:14].[Na+].[OH-].[Na+].Cl[O-].[Na+].S([O-])([O-])=S.[Na+].[Na+].Cl>CO>[I:14][C:5]1[CH:6]=[C:1]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:2]=[CH:3][C:4]=1[OH:7]

참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 71034-HydroxybiphenylHCID 14798Sodium HydroxideHCID 15847209sodium thiosulfite anhydrousHCID 23665760Sodium Hypochlorite

생성물 1

HCID 41061404-Hydroxy-3-iodobiphenyl

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
0 °C

실험 절차

Biphenyl-4-ol((5.26 g, 30.9 mmol), sodium iodide (4.635 g, 30.9 mmol), sodium hydroxide (1.276 g, 31.9 mmol) was dissolved in methanol (85 mL) and cooled to 0° C. To the solution was added 12% (w/v) sodium hypochlorite (20 mL) dropwise maintaining the temperature below 4° C. The solution was stirred at this temperature for 1 hour and then 2M sodium thiosulfite (50 mL) wad added and the pH of the solution was adjusted to >pH 7 with 1M HCl. The mixture was filtered and the filtrate was washed with water. The solid was dried in a vacuum oven and then the title product was obtained as crystals after recrystallisation from heptane. Yield 7.08 g, 77%.

후처리

  1. temperaturedropwise maintaining the temperature below 4° C
  2. filtrationThe mixture was filtered
  3. washthe filtrate was washed with water
  4. customThe solid was dried in a vacuum oven

출처 및 근거

ORD 기록
ord-015dc7f31fe34963ae9cf14d583f1eee
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612068B2

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