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

HRID 5755

반응식

HRID 5755 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-1d8e39248edc4f098a636d77133a05dd
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05246747

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