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

HRID 1734601
ノート
印刷プレビュー

反応式

HRID 1734601 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 540198812-Amino-5-ethynyl-6-methylbenzonitrile収率 106.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7ba055e518d6411fb46fd33f595eb5a5
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05534518

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート