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2-Amino-4-bromopyridine-3-carbonitrile → 7-Bromo-3-(2,2,2-trifluoro-ethyl)-imidazo[1,2-a]pyridine-8-carbonitrile

HRID 2361744
ノート
印刷プレビュー

反応式

HRID 2361744 の反応式
[NH2:1][C:2]1[N:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:3]=1[C:4]#[N:5].Br[CH:12]([CH2:15][C:16]([F:19])([F:18])[F:17])[CH:13]=O>CCO.CCOC(C)=O>[Br:10][C:6]1[CH:7]=[CH:8][N:9]2[C:12]([CH2:15][C:16]([F:19])([F:18])[F:17])=[CH:13][N:1]=[C:2]2[C:3]=1[C:4]#[N:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 580811212-Amino-4-bromopyridine-3-carbonitrileHCID 580811402-Bromo-4,4,4-trifluorobutyraldehyde

生成物 1

HCID 580811287-Bromo-3-(2,2,2-trifluoro-ethyl)-imidazo[1,2-a]pyridine-8-carbonitrile収率 48.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
150 °C

実験手順

A mixture of compounds D8 (2 g, 10.1 mmol) and D4 (2.898 g, 14.14 mmol) in EtOH (10 ml) was subjected to microwave heating at 150° C. for 40 min. After cooling to room temperature, the solvent was evaporated in vacuo. The residue thus obtained was diluted with EtOAc and washed with water. The organic layer was separated and washed with water, then with 1M HCl (aqueous solution), dried (MgSO4) and evaporated in vacuo. The crude product thus obtained was triturated with diethylether to yield compound D9 (1.5 g, 48.8%).

後処理

  1. temperatureAfter cooling to room temperature
  2. customthe solvent was evaporated in vacuo
  3. customThe residue thus obtained
  4. washwashed with water
  5. customThe organic layer was separated
  6. washwashed with water
  7. dry with materialwith 1M HCl (aqueous solution), dried (MgSO4)
  8. customevaporated in vacuo
  9. customThe crude product thus obtained
  10. customwas triturated with diethylether

出典と根拠

ORDレコード
ord-4f1da4511e3c44189c88ec8c78263079
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08691813B2

反応ノート

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