Triethylamine → HCID 70222494, 화합물

HRID 1532457

반응식

HRID 1532457 반응식
[C:1]1([S:7]([CH2:10][CH2:11]O)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CS(OS(C)(=O)=O)(=O)=O.C(N(CC)CC)C.I[C:30]1[CH:35]=[CH:34][C:33]([O:36][CH2:37][CH3:38])=[CH:32][CH:31]=1.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(#N)C>[C:1]1([S:7]([CH:10]=[CH:11][C:30]2[CH:35]=[CH:34][C:33]([O:36][CH2:37][CH3:38])=[CH:32][CH:31]=2)(=[O:8])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 302022-(Phenylsulfonyl)ethanolHCID 80271Tri-o-tolylphosphineHCID 81560Methanesulfonic anhydrideHCID 2207001-Ethoxy-4-iodobenzene

생성물 1

HCID 70222494HCID 70222494, 화합물수율 55%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 6342Acetonitrile용매

반응 조건

온도
50 °C

실험 절차

To 0.186 g (1.0 mmol) of 2-(phenylsulfonyl)ethanol, 3 ml of acetonitrile was added, followed by 0.19 g (1.1 mmol) of methanesulfonic anhydride and 0.56 ml (4.0 mmol) of triethylamine, and the mixture was stirred for 5 hours at the internal temperature of 50° C. Subsequently, 0.37 g (1.5 mmol) of p-iodophenetole, 0.011g (0.05 mmol) of palladium acetate, and 0.067 g (0.22 mmol) of tri(o-tolyl)phosphine were added thereto, and the mixture was then refluxed for 17 hours. After cooled to room temperature, the reaction mixture was concentrated and purified by column chromatography (hexane/ethyl acetate=80/20) to obtain 0.158 g of [2-(phenylsulfonyl)ethenyl]-4-ethoxybenzene. Yield: 55%.

후처리

  1. temperaturethe mixture was then refluxed for 17 hours
  2. temperatureAfter cooled to room temperature
  3. concentrationthe reaction mixture was concentrated
  4. custompurified by column chromatography (hexane/ethyl acetate=80/20)

출처 및 근거

ORD 기록
ord-8880cbe823044e85aa36ca7dbbc725ae
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06201131B1

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