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Aniline → Bis-(6-bromo-hexyl)-phenyl-amine

HRID 599135
ノート
印刷プレビュー

反応式

HRID 599135 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH:9]([Br:15])[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[C:16]([O-])(=O)[CH3:17].[Na+]>O>[Br:15][CH2:9][CH2:10][CH2:11][CH2:12][CH2:16][CH2:17][N:1]([CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][Br:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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 3

HCID 6115AnilineHCID 517045Sodium AcetateHCID 118068541,1-Dibromohexane

生成物 1

HCID 67270812Bis-(6-bromo-hexyl)-phenyl-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
97.5 °C

実験手順

0.45 ml of aniline (5 mmol), 2.5 ml of dibromohexane (14.6 mmol), and sodium acetate (14.5 mmol) were charged in a reaction container and slowly heated to about 95 to 100° C. while generating bubbles under a nitrogen atmosphere. The reactant mixture was agitated for about 10 hours at about 95 to 100° C. The mixture was cooled down to room temperature, mixed with 30 ml of distilled water, and agitated for 10 minutes. The mixture was then treated to extract organic layers using ethylacetate, and then was distillated through reduced pressure distillation, thereby obtaining a sticky liquid. The sticky liquid was separated using preparative TLC (eluent: CH2Cl2:Hexane=1:2.5). The obtained compound was confirmed to be the compounds 221 of FIG. 3 using a 1H-NMR spectometry and mass spectometry. The results are shown in FIG. 5.

後処理

  1. temperatureThe mixture was cooled down to room temperature
  2. stirringagitated for 10 minutes
  3. additionThe mixture was then treated
  4. extractionto extract organic layers
  5. distillationwas distillated through reduced pressure distillation
  6. customobtaining a sticky liquid
  7. customThe sticky liquid was separated

出典と根拠

ORDレコード
ord-5d7d5fa79147443780191fa2d7ccd7fe
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897735B2

反応ノート

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