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Water → 1-(4-n-Butylphenylethynyl)-4-(4-n-propylphenylethynyl)naphthalene

HRID 403067
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HRID 403067 반응식
BrC1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]#[C:13][C:14]2[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][CH3:22])=[CH:16][CH:15]=2)=[CH:4]C=1.[CH2:23]([C:27]1[CH:32]=[CH:31][C:30]([C:33]#[CH:34])=[CH:29][CH:28]=1)[CH2:24][CH2:25][CH3:26].O.[CH3:36][CH2:37]CCCCC>CCN(CC)CC.[Cu]I.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>[CH2:33]([C:30]1[CH:29]=[CH:28][C:27]([C:23]#[C:24][C:25]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]([C:12]#[C:13][C:14]3[CH:15]=[CH:16][C:17]([CH2:20][CH2:21][CH3:22])=[CH:18][CH:19]=3)=[CH:4][CH:26]=2)=[CH:32][CH:31]=1)[CH2:34][CH2:36][CH3:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962WaterHCID 8900HeptaneHCID 27751321-Butyl-4-ethynylbenzeneHCID 671178511-Bromo-4-(4-n-propylphenylethynyl)naphthalene

생성물 1

HCID 867624711-(4-n-Butylphenylethynyl)-4-(4-n-propylphenylethynyl)naphthalene

시약·촉매·용매 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 178418476HCID 178418476, 화합물촉매
HCID 8471Triethylamine용매

실험 절차

2.35 g (6.3 mmol) of 1-bromo-4-(4-n-propylphenylethynyl)naphthalene and 1.33 g (8.4 mmol) of 4-n-butylphenylacetylene are initially introduced in 40 ml of NEt3, 60 mg (0.3 mmol) of copper(I) iodide and 200 mg (0.3 mmol) of bis(triphenylphosphine)palladium(II) chloride are added, and the mixture is refluxed for 18 h. The batch is cooled, water and heptane are added, and the phases are separated. The organic phase is washed with saturated ammonium chloride solution and subsequently with saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated in a rotary evaporator. The residue of compound (1) is purified by column chromatography (SiO2, heptane), and the further purification is carried out by recrystallisation from isopropanol.

후처리

  1. temperaturethe mixture is refluxed for 18 h
  2. temperatureThe batch is cooled
  3. customthe phases are separated
  4. washThe organic phase is washed with saturated ammonium chloride solution and subsequently with saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated in a rotary evaporator
  8. customThe residue of compound (1) is purified by column chromatography (SiO2, heptane)
  9. customthe further purification
  10. customis carried out by recrystallisation from isopropanol

출처 및 근거

ORD 기록
ord-c8d6a1e4633540f19073da98de7a307e
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08747695B2

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