Tributylstannane → HCID 22262058, 화합물

HRID 1610763노트

반응식

HRID 1610763 반응식
Br[C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[O:9][CH2:10][C:11]([CH3:13])=[CH2:12].N(C(C)(C)C#N)=NC(C)(C)C#N.C([SnH](CCCC)CCCC)CCC>C1(C)C=CC=CC=1>[CH3:12][C:11]1([CH3:13])[C:2]2[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=2[O:9][CH2:10]1

참가 물질

5

반응물 3

HCID 5948TributylstannaneHCID 6547AzobisisobutyronitrileHCID 334095HCID 334095, 화합물

생성물 1

HCID 22262058HCID 22262058, 화합물수율 110.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of 2-bromo-4-methyl-1-[(2-methyl-2-propenyl)oxy]benzene (5.0 g, 20.7 mmol) in toluene (100 ml) were added 2,2′-azobisisobutyronitrile (1.45 g, 8.8 mmol) and tri-n-butyltin hydride (8.34 ml, 31 mmol), and the mixture was heated under reflux overnight. After completion of the reaction, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:0, 50:1) to give 3,3,5-trimethyl-2,3-dihydro-1-benzofuran (3.70 g, 100%) as a colorless transparent oil.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux overnight
  3. customAfter completion of the reaction
  4. customthe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:0, 50:1)

출처 및 근거

ORD 기록
ord-50dc93ea35f742898aceb3aca3d48cff
출처 데이터셋
uspto-grants-2006_01
특허 번호
US06982348B2

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