Triethylamine → (4-Methoxymethoxy-phenylethynyl)-trimethylsilane

HRID 2305607

반응식

HRID 2305607 반응식
I[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][O:10][CH3:11])=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:19][Si:20]([C:23]#[CH:24])([CH3:22])[CH3:21]>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu](I)I.O.C(OCC)(=O)C>[CH3:19][Si:20]([CH3:22])([CH3:21])[C:23]#[C:24][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][O:10][CH3:11])=[CH:4][CH:3]=1

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 66111TrimethylsilylacetyleneHCID 110327301-Iodo-4-(methoxymethoxy)benzene

생성물 1

HCID 10657368(4-Methoxymethoxy-phenylethynyl)-trimethylsilane

시약·촉매·용매 3

HCID 83717Copper iodide촉매HCID 178418476HCID 178418476, 화합물촉매HCID 22728543Water ethylacetate용매

실험 절차

5.74 g (21.7 mmol) of 1-iodo-4-methoxymethoxybenzene, 100 ml of triethylamine and a mixture of 1.53 g (2.18 mmol) of dichlorobis(triphenylphosphine)palladium and 831 mg (4.37 mmol) of copper iodide are introduced into a three-necked flask. 6.14 ml (43.5 mmol) of trimethylsilylacetylene are then added and the medium is stirred for 48 h at room temperature. It is then poured into a water/ethyl acetate mixture. The organic phase is washed twice with water and, after separation of the phases by settling, it is washed with magnesium sulphate and concentrated.

후처리

  1. additionare introduced into a three-necked flask
  2. washThe organic phase is washed twice with water
  3. customafter separation of the phases
  4. washit is washed with magnesium sulphate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-107dc54a56b3407990ed501fdd2fb309
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06441010B2

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