Ammonia → 2-(4-Iodophenyl)ethan-1-ol

HRID 735023

반응식

HRID 735023 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][OH:10])=[CH:4][CH:3]=1.[I-:11].[Na+].NCCN.N>[Cu]I.O.O1CCOCC1>[I:11][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][OH:10])=[CH:4][CH:3]=1

참가 물질

8

반응물 4

HCID 222AmmoniaHCID 3301EthylenediamineHCID 5238Sodium IodideHCID 728512-(4-Bromophenyl)ethanol

생성물 1

HCID 30407702-(4-Iodophenyl)ethan-1-ol

시약·촉매·용매 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

0.474 g (2.48 mmol) of copper (I) iodide, 5 g (24.86 mmol 2-(4-bromophenyl)ethanol and 7.45 g (49.73 mmol) of sodium iodide are successively added to a flask under an argon atmosphere. Then 0.438 g (4.97 mmol) of dimethylenediamine and 25 mL dioxane are added and the reaction mixture is refluxed for 14 hours. Then the reaction mixture is combined with 20 mL concentrated ammonia solution at ambient temperature, with 100 mL of water diluted and extracted with dichloromethane. The organic phase is extracted three times with water and dried over sodium sulfate. Yield: 5.4 g (87.5% of theory); C8H9IO (M=248.06); calc.: molecular ion peak (M)+: 248; found: molecular ion peak (M)+: 248; Rf value: 0.6 (silica gel, dichloromethane/ethanol (10:1)).

후처리

  1. temperaturethe reaction mixture is refluxed for 14 hours
  2. additiondiluted
  3. extractionextracted with dichloromethane
  4. extractionThe organic phase is extracted three times with water
  5. dry with materialdried over sodium sulfate

출처 및 근거

ORD 기록
ord-ba01858f6ae24ea0847813801ff18e2e
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07592373B2

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