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Sodium Hydroxide → 1-(2,4-Dichlorophenyl)-1-(2,4-dichlorophenoxyethoxy)-2-(1,2,4-triazol-1-yl)-1-ethanol

HRID 622402
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HRID 622402 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([OH:16])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.[OH-:17].[Na+].[Cl:19][C:20]1[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:21]=1[O:22][CH2:23][CH2:24]Br>C1(C)C=CC=CC=1.[Cl-].C([N+](CCCCCCCCCCCC)(C)C)C1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]([O:17][CH2:24][CH2:23][O:22][C:21]1[CH:26]=[CH:27][C:28]([Cl:30])=[CH:29][C:20]=1[Cl:19])([OH:16])[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1
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참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 1388811-(2-Bromoethoxy)-2,4-dichlorobenzeneHCID 66285758905-18-3

생성물 1

HCID 540910161-(2,4-Dichlorophenyl)-1-(2,4-dichlorophenoxyethoxy)-2-(1,2,4-triazol-1-yl)-1-ethanol수율 35%

시약·촉매·용매 2

HCID 8753Benzododecinium Chloride촉매
HCID 1140
Toluene
용매

실험 절차

12.95 g (0.05 mole) of 1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-1-ethanol are dissolved in 100 ml of toluene, and 100 ml of 40% strength sodium hydroxide solution and 1 ml of benzyl-dodecyl-dimethylammonium chloride are added. 13.5 g (0.05 mole) of 2,4-dichlorophenoxyethyl bromide are then added dropwise and the mixture is subsequently stirred at room temperature for 48 hours. The organic phase is separated off, washed with three 100 ml portions of saturated sodium chloride solution, dried over sodium sulphate and concentrated. The residue is taken up in 100 ml of diethyl ether, and crystallizes after the mixture has stood for a short time. 7.8 g (35% of theory) of 1-(2,4-dichlorophenyl)-1-(2,4-dichlorophenoxyethoxy)-2-(1,2,4-triazol-1-yl)-1-ethanol of melting point 88°-90° C. are obtained.

후처리

  1. customThe organic phase is separated off
  2. washwashed with three 100 ml portions of saturated sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated
  5. customcrystallizes after the mixture

출처 및 근거

ORD 기록
ord-d7a727d7bc5a4a128c7380354907e17c
출처 데이터셋
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04771065

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