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

HRID 52639
ノート
印刷プレビュー

反応式

HRID 52639 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-6ca0f8cf077743da931057d9eaae1df2
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05616718

反応ノート

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