Triethylamine → 1-(2-Chlorophenyl)-4-{2-[bis(4-hydroxyphenyl)methyl]benzyl}piperazine

HRID 36444

반응식

HRID 36444 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.C(N(CC)CC)C.[OH:21][C:22]1[CH:27]=[CH:26][C:25]([CH:28]([C:37]2[CH:42]=[CH:41][C:40]([OH:43])=[CH:39][CH:38]=2)[C:29]2[CH:36]=[CH:35][CH:34]=[CH:33][C:30]=2[CH2:31]Br)=[CH:24][CH:23]=1>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:13][CH2:12][N:11]([CH2:31][C:30]2[CH:33]=[CH:34][CH:35]=[CH:36][C:29]=2[CH:28]([C:25]2[CH:24]=[CH:23][C:22]([OH:21])=[CH:27][CH:26]=2)[C:37]2[CH:42]=[CH:41][C:40]([OH:43])=[CH:39][CH:38]=2)[CH2:10][CH2:9]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 4156281-(2-Chlorophenyl)piperazineHCID 199381762-[Bis(4-hydroxyphenyl)methyl]benzylbromide

생성물 1

HCID 199381181-(2-Chlorophenyl)-4-{2-[bis(4-hydroxyphenyl)methyl]benzyl}piperazine수율 14.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In 50 ml of tetrahydrofuran were dissolved 1.5 g of 1-(2-chlorophenyl)piperazine and 5 ml of triethylamine, and 3.4 g of 2-[bis(4-hydroxyphenyl)methyl]benzylbromide was added thereto. The mixture was heated under reflux for 3.5 hours, and then insoluble substances were filtered off. The filtrate was concentrated, and the residue was subjected to extraction with the addition of water and ethyl acetate. The organic layer was separated, and the aqueous layer was then extracted with ethyl acetate. The organic layers were combined and then dried over anhydrous magnesium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by silica gel chromatography to afford 0.54 g of the desired compound (Compound 89).

후처리

  1. additionwas added
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 3.5 hours
  4. filtrationinsoluble substances were filtered off
  5. concentrationThe filtrate was concentrated
  6. extractionthe residue was subjected to extraction with the addition of water and ethyl acetate
  7. customThe organic layer was separated
  8. extractionthe aqueous layer was then extracted with ethyl acetate
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customThe solvent was evaporated off under reduced pressure
  11. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-0208c64273a84e8e8c4fda96508a2f39
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05413997

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