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Cyanogen Bromide → HCID 86626274, 화합물

HRID 1097549
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HRID 1097549 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10476Cyanogen BromideHCID 117470392-Chloro-N4-(2-methylpropyl)-3,4-quinolinediamine

생성물 1

HCID 86626274HCID 86626274, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a198fe4280b4467b9588fb7e93c36643
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08143270B2

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