Acetyl chloride → n-(4-Amino-5-cyano-6-ethylpyridin-2-yl)acetamide

HRID 1364534ノート

反応式

HRID 1364534 の反応式
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH2:10][CH3:11])[N:5]=[C:4]([NH2:12])[CH:3]=1.[C:13](Cl)([CH3:15])=[O:14]>N1C=CC=CC=1>[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH2:10][CH3:11])[N:5]=[C:4]([NH:12][C:13](=[O:14])[CH3:15])[CH:3]=1

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 451224114,6-Diamino-2-ethyl-nicotinonitrile

生成物 1

HCID 66920553n-(4-Amino-5-cyano-6-ethylpyridin-2-yl)acetamide収率 68%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

The 4,6-diamino nicotinonitrile from Example 101A (35 mg, 0.22 mmol) was dissolved in 0.5 mL of anhydrous pyridine. AcCl was then dropped in until the TLC shows the starting material was completely consumed (appr. 150 μL of AcCl used). Water was then added, the light-yellow precipitate was collected through filtration and dried in vacuum oven to provide the titled compound (30 mg, 68% yield). 1H NMR (300 MHz, DMSO-d6) δ 10.28 (s, 1H), 7.39 (s, 1H), 6.82 (s, 2H), 2.66 (q, J=7.5 Hz, 2H), 2.06 (s, 3H), 1.19 (t, J=7.5 Hz, 3H). MS (ESI) m/e 205 (M+H)+.

後処理

  1. customwas completely consumed (appr. 150 μL of AcCl used)
  2. additionWater was then added
  3. filtrationthe light-yellow precipitate was collected through filtration
  4. customdried in vacuum oven

出典と根拠

ORDレコード
ord-af22593d54de447992803a4fa80028ad
出典データセット
uspto-grants-2011_02
特許番号
US07888374B2

反応ノート

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