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Imidazole → HCID 67345597、化合物

HRID 882086
ノート
印刷プレビュー

反応式

HRID 882086 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([C:15]#[N:16])[C:11]=1[N:12]([CH3:14])[CH3:13])[N:8]=[C:7]([CH2:17][OH:18])[CH:6]=[CH:5]2.[CH3:19][C:20]([Si:23](Cl)([CH3:25])[CH3:24])([CH3:22])[CH3:21].N1C=CN=C1>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([C:15]#[N:16])[C:11]=1[N:12]([CH3:14])[CH3:13])[N:8]=[C:7]([CH2:17][O:18][Si:23]([C:20]([CH3:22])([CH3:21])[CH3:19])([CH3:25])[CH3:24])[CH:6]=[CH:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 67324605HCID 67324605、化合物

生成物 1

HCID 67345597HCID 67345597、化合物収率 69.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The 6-bromo-7-dimethylamino-2-(hydroxymethyl)quinoline-8-carbonitrile (2 g, 6.5 mmol, 1 eq), TBDMSCl (1.4 g, 7.3 mmol, 1.1 eq) and imidazole (623 mg, 7.3 mmol, 1.1 eq) were added to DMF (20 mL). The resulting solution was stirred at room temperature for 3 hours, and then the solvent was removed under high reduced pressure. Cyclohexane was added and the mixture was washed twice with water, and then with brine. The organic layer was then dried over MgSO4, and concentrated under reduced pressure. The product was obtained pure as a yellow powder (1.9 g, 68%).

後処理

  1. customthe solvent was removed under high reduced pressure
  2. additionCyclohexane was added
  3. washthe mixture was washed twice with water
  4. dry with materialThe organic layer was then dried over MgSO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-185d4300115d4f52b89b0b70901554fa
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993767B2

反応ノート

読み込み中…

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