Potassium Carbonate → 2-Amino-3-cyano-4-methyl-5-ethynylpyridine

HRID 1078242ノート

反応式

HRID 1078242 の反応式
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH3:10])[C:5]([C:11]#[C:12][Si](C)(C)C)=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+]>CO>[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH3:10])[C:5]([C:11]#[CH:12])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 197071982-Amino-3-cyano-4-methyl-5-(trimethylsilylethynyl)pyridine

生成物 1

HCID 233567022-Amino-3-cyano-4-methyl-5-ethynylpyridine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2.8 grams (0.012 mole) of 2-amino-3-cyano-4-methyl-5-(trimethylsilylethynyl)pyridine and 1.8 grams (0.012 mole) of potassium carbonate in 100 mL of methanol is stirred at ambient temperature for one hour. The reaction mixture is then concentrated under reduced pressure to a residue. The residue is taken up in about 150 mL of water, and the solution is extracted with two 250 mL portions of diethyl ether. The combined extracts are dried with magnesium sulfate and filtered. The filtrate is concentrated under reduced pressure, yielding 2-amino-3-cyano-4-methyl-5-ethynylpyridine.

後処理

  1. concentrationThe reaction mixture is then concentrated under reduced pressure to a residue
  2. extractionthe solution is extracted with two 250 mL portions of diethyl ether
  3. dry with materialThe combined extracts are dried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate is concentrated under reduced pressure

出典と根拠

ORDレコード
ord-47c5237d19ec4855aa10deed945195a6
出典データセット
uspto-grants-1996_08
特許番号
US05547954

反応ノート

読み込み中…