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Potassium Fluoride → HCID 15811458, 화합물

HRID 556141
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HRID 556141 반응식
C[Si]([C:5]#[C:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[CH:18]=[CH:17][C:16]([C:19]#[C:20][Si](C)(C)C)=[CH:15][N:14]=2)=[N:11][CH:12]=1)(C)C.[F-].[K+]>CO>[C:19]([C:16]1[CH:17]=[CH:18][C:13]([C:10]2[CH:9]=[CH:8][C:7]([C:6]#[CH:5])=[CH:12][N:11]=2)=[N:14][CH:15]=1)#[CH:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 522689Potassium FluorideHCID 52476625,5'-Bis(trimethylsilylethynyl)-2,2'-bipyridine

생성물 1

HCID 15811458HCID 15811458, 화합물수율 85.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Subsequently, the obtained 5,5′-bis(trimethylsilylethynyl)-2,2′-bipyridyl (120 mg, 0.34 mmol) and potassium fluoride (KF: 42 mg, 0.72 mmol) were added with dist. methanol (MeOH: 12 mL). The resultant mixture was then stirred under a nitrogen atmosphere at room temperature for 11 hours to obtain a reaction mixture. After that, an organic layer in the reaction mixture was then concentrated to obtain a crude product (II). Subsequently, the obtained crude product (II) was separated and purified by silica gel column chromatography (CH2Cl2=100) to obtain 5,5′-diethynyl-2,2′-bipyridyl (59.5 mg, 85% yield (in two steps)).

후처리

  1. customto obtain a reaction mixture
  2. concentrationAfter that, an organic layer in the reaction mixture was then concentrated
  3. customto obtain a crude product (II)
  4. customSubsequently, the obtained crude product (II)
  5. customwas separated
  6. custompurified by silica gel column chromatography (CH2Cl2=100)

출처 및 근거

ORD 기록
ord-d8eb6f44f47f480fb4c8db71a8ae96af
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08053588B2

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