Iodine → 2-iodobenzene-1,3-diol

HRID 1064738노트

반응식

HRID 1064738 반응식
[C:1]1([CH:8]=[CH:7][CH:6]=[C:4]([OH:5])[CH:3]=1)[OH:2].[I:9]I.C([O-])(O)=O.[Na+]>O>[I:9][C:3]1[C:1]([OH:2])=[CH:8][CH:7]=[CH:6][C:4]=1[OH:5]

참가 물질

5

반응물 3

HCID 807IodineHCID 5054ResorcinolHCID 516892Sodium Bicarbonate

생성물 1

HCID 6168332-iodobenzene-1,3-diol수율 78%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Resorcinol (2.75 g, 25 mmol) in 20 mL of water and ice was treated with iodine (6.7 g, 26.4 mmol) and NaHCO3 (2.3 g, 27.4 mmol) in one portion. After stirring for 1 hour, the precipitate was separated by filtration and the filtrate was extracted twice (2×75 mL) with diethyl ether. The organic phase was dried over sodium sulfate and evaporated under reduced pressure. The solid was triturated with 20 ML of chloroform and left at −18° C. for 24 hours. The solid was separated by filtration to provide the title compound (78% yield). 1HNMR (300 MHz, CDCl3) δ 4.85 (s, 1H), 6.30 (m, 2H), 6.95 (m, 1H). MS (CDI) m/z 237 (M+H)+.

후처리

  1. customthe precipitate was separated by filtration
  2. extractionthe filtrate was extracted twice (2×75 mL) with diethyl ether
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. customevaporated under reduced pressure
  5. customThe solid was triturated with 20 ML of chloroform
  6. waitleft at −18° C. for 24 hours
  7. customThe solid was separated by filtration

출처 및 근거

ORD 기록
ord-de040ce6123e477ab7fc3b605a4116d5
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969730B2

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