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Potassium Carbonate → 2-Amino-5-ethynyl-6-methylbenzonitrile

HRID 1734601
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HRID 1734601 반응식
[NH2:1][C:2]1[CH:9]=[CH:8][C:7]([C:10]#[C:11][Si](C)(C)C)=[C:6]([CH3:16])[C:3]=1[C:4]#[N:5].C(=O)([O-])[O-].[K+].[K+]>CO>[NH2:1][C:2]1[CH:9]=[CH:8][C:7]([C:10]#[CH:11])=[C:6]([CH3:16])[C:3]=1[C:4]#[N:5]
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참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 543680762-Amino-5-(trimethylsilylethynyl)-6-methylbenzonitrile

생성물 1

HCID 540198812-Amino-5-ethynyl-6-methylbenzonitrile수율 106.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 1.4 grams (0.006 mole) of 2-amino-5-(trimethylsilylethynyl)-6-methylbenzonitrile and 0.9 gram (0.006 mole) of potassium carbonate in 50 mL of methanol was stirred at ambient temperature for one hour. The reaction mixture was then concentrated under reduced pressure to a residue. The residue was taken up in about 75 mL of water, and the solution was extracted with two 200 mL portions of diethyl ether. The combined extracts were dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure, yielding 1.0 gram of 2-amino-5-ethynyl-6-methylbenzonitrile. The NMR spectrum was consistent with the proposed structure. This reaction was repeated several times.

후처리

  1. concentrationThe reaction mixture was then concentrated under reduced pressure to a residue
  2. extractionthe solution was extracted with two 200 mL portions of diethyl ether
  3. dry with materialThe combined extracts were dried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7ba055e518d6411fb46fd33f595eb5a5
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05534518

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