2-(Dimethylamino)ethanol → 10-[4-[[4-(dodecyl)phenyl]azo]phenoxy]-N-(2-hydroxyethyl)-N,N-dimethyl-1-decanaminium bromide

HRID 5755

反応式

HRID 5755 の反応式
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([N:19]=[N:20][C:21]2[CH:26]=[CH:25][C:24]([CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH3:38])=[CH:23][CH:22]=2)=[CH:15][CH:14]=1.[CH3:39][N:40]([CH3:44])[CH2:41][CH2:42][OH:43].O1CCCC1>CO>[Br-:1].[CH2:27]([C:24]1[CH:25]=[CH:26][C:21]([N:20]=[N:19][C:16]2[CH:17]=[CH:18][C:13]([O:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][N+:40]([CH2:41][CH2:42][OH:43])([CH3:44])[CH3:39])=[CH:14][CH:15]=2)=[CH:22][CH:23]=1)[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH3:38]

参加物

5

反応物 3

HCID 79022-(Dimethylamino)ethanolHCID 8028TetrahydrofuranHCID 197929294-(10-Bromodecyloxy)-4'-dodecylazobenzene

生成物 1

HCID 1979292710-[4-[[4-(dodecyl)phenyl]azo]phenoxy]-N-(2-hydroxyethyl)-N,N-dimethyl-1-decanaminium bromide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 3000 ml three-necked round bottom flask was equipped with magnetic stirring, a heating mantle, a reflux condenser, and a nitrogen atmosphere. The flask was charged with 4-(10-bromodecyloxy)-4'-dodecylazobenzene (40 g, 0.068 mol), dimethylethanolamine (95.2 g, 1.068 mole) and 1050 ml of tetrahydrofuran. The reaction mixture was allowed to reflux for 24 hours. During the course of the reaction mixture. After 24 hours, the reaction mixture was cooled to room temperature, and then chilled in an icewater bath. The crystalline solid was isolated by suction filtration. The crude product was dissolved in hot methanol and filtered to remove insoluble impurities. The methanol was removed by evaporation at reduced pressure The crude product was recrystallized from tetrahydrofuran. Yield 28.0 g, 61.0%.

後処理

  1. customA 3000 ml three-necked round bottom flask was equipped with magnetic stirring
  2. temperatureto reflux for 24 hours
  3. temperaturechilled in an icewater bath
  4. customThe crystalline solid was isolated by suction filtration
  5. filtrationfiltered
  6. customto remove insoluble impurities
  7. customThe methanol was removed by evaporation at reduced pressure The crude product
  8. customwas recrystallized from tetrahydrofuran

出典と根拠

ORDレコード
ord-1d8e39248edc4f098a636d77133a05dd
出典データセット
uspto-grants-1993_09
特許番号
US05246747

関連ノート

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