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Cyanogen Bromide → HCID 86626274、化合物

HRID 1097549
ノート
印刷プレビュー

反応式

HRID 1097549 の反応式
[Cl:1][C:2]1[C:11]([NH2:12])=[C:10]([NH:13][CH2:14][CH:15]([CH3:17])[CH3:16])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[N:18]#[C:19][Br:20]>C(O)C>[BrH:20].[Cl:1][C:2]1[C:11]2[N:12]=[C:19]([NH2:18])[N:13]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1
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 10476Cyanogen BromideHCID 117470392-Chloro-N4-(2-methylpropyl)-3,4-quinolinediamine

生成物 1

HCID 86626274HCID 86626274、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-chloro-N4-(2-methylpropyl)-3,4-quinolinediamine (André et al, U.S. Pat. No. 4,988,815, Example 6, 8.92 g, 35.7 mmol) in ethanol (50 mL) was stirred at 100° C.; cyanogen bromide (5.67 g, 53.5 mmol) was added in one portion. The red solution was stirred overnight, washed three times with water, and washed once with brine. A precipitate formed in the aqueous washings and was isolated by filtration. The organic fraction was dried over magnesium sulfate, filtered through a layer of CELITE filer agent, concentrated under reduced pressure, further dried under high vacuum, and combined with the isolated precipitate to provide 9.81 g of 4-chloro-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinoline-2-amine hydrobromide as a dark red solid.

後処理

  1. washwashed three times with water
  2. washwashed once with brine
  3. customA precipitate formed in the aqueous washings
  4. customwas isolated by filtration
  5. dry with materialThe organic fraction was dried over magnesium sulfate
  6. filtrationfiltered through a layer of CELITE filer agent
  7. concentrationconcentrated under reduced pressure
  8. customfurther dried under high vacuum

出典と根拠

ORDレコード
ord-a198fe4280b4467b9588fb7e93c36643
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08143270B2

反応ノート

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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