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Triethylamine → {3-[3-(2-Methoxy-ethyl)-cyclobutyl]-phenylethynyl}-triisopropyl-silane

HRID 2240966
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HRID 2240966 반응식
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH:8]2[CH2:11][CH:10]([CH2:12][CH2:13][O:14][CH3:15])[CH2:9]2)[CH:3]=1.[CH:16]([Si:19]([C:26]#[CH:27])([CH:23]([CH3:25])[CH3:24])[CH:20]([CH3:22])[CH3:21])([CH3:18])[CH3:17].C(N(CC)CC)C>[Cu](I)I.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:15][O:14][CH2:13][CH2:12][CH:10]1[CH2:11][CH:8]([C:4]2[CH:3]=[C:2]([C:27]#[C:26][Si:19]([CH:16]([CH3:18])[CH3:17])([CH:23]([CH3:25])[CH3:24])[CH:20]([CH3:22])[CH3:21])[CH:7]=[CH:6][CH:5]=2)[CH2:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 2734682(Triisopropylsilyl)acetyleneHCID 593053151-Bromo-3-[3-(2-methoxy-ethyl)-cyclobutyl]-benzene

생성물 1

HCID 59305302{3-[3-(2-Methoxy-ethyl)-cyclobutyl]-phenylethynyl}-triisopropyl-silane수율 90.3%

시약·촉매·용매 2

HCID 83717Copper iodide촉매
HCID 178418397
HCID 178418397, 화합물
촉매

실험 절차

In a CEM snap top microwave vial were combined 1-Bromo-3-[3-(2-methoxy-ethyl)-cyclobutyl]-benzene (0.340 gm 1.28 mmol), triisopropylsilylacetylene (0.29 g, 1.12 mmol), copper iodide (9 mg, 0.178 mmol), tetrakis(triphenylphosphine)palladium (29 mg, 0.088 mmol) and triethylamine (1.30 g, 12.8 mmol). The vial was quickly agitated then irradiated in a CEM Explorer™ microwave instrument for 30 minutes at 80° C. Purification by column chromatography (hexanes) afforded an oil 375 mg (80%). This material was used in next step without further characterization.

후처리

  1. customthen irradiated in a CEM Explorer™ microwave instrument for 30 minutes at 80° C
  2. customPurification by column chromatography (hexanes)

출처 및 근거

ORD 기록
ord-6172c194434a46a2974d92dffd81535c
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07723368B2

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