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Hydrochloric Acid → HCID 18966366, 화합물

HRID 2226108
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HRID 2226108 반응식
C([Li])CCC.[CH3:6][O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[N:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=2)[CH2:16][CH2:15]1.[CH:28](=[O:37])[C:29]1[C:30]([O:35][CH3:36])=[CH:31][CH:32]=[CH:33][CH:34]=1.Cl>C1COCC1.C(O)(C)C.O>[CH3:6][O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[N:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][C:22]2[C:27]([CH:28]([OH:37])[C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[O:35][CH3:36])=[CH:26][CH:25]=[CH:24][N:23]=2)[CH2:16][CH2:15]1
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 86582-MethoxybenzaldehydeHCID 199286Piperazine, 1-(o-methoxyphenyl)-4-(2-(2-pyridyl)ethyl)-HCID 178418339Butyllithium

생성물 1

HCID 18966366HCID 18966366, 화합물

시약·촉매·용매 3

HCID 962Water용매
HCID 3776
Isopropanol
용매
HCID 8028Tetrahydrofuran용매2회

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온도
-70 °C

실험 절차

n-Butyl-lithium (1.6M solution in hexane) (7.0 ml, 11.2 mmol, 1.1 equiv.) was added dropwise at below -60° C. to a solution of 1-(2-methoxyphenyl)-4-(2-pyridylethyl)piperazine base (3.00 g, 10.1 mmol) in anhydrous THF (20 ml). The resulting orange-red solution was stirred for a further 0.25 h at -70° C. then quenched with a solution of ortho-anisaldehyde (1.5 g, 11.0 mmol) in anhydrous THF (2 ml). The reaction mixture was poured into water (50 ml) and extracted with dichloromethane (2×75 ml). The organic extract was washed (brine), dried (Na2SO4) and concentrated in vacuo. The residue was subjected to chromatography (SiO2 :Et2O) to give the first Rf diastereoisomer as a white foam which was dissolved in isopropanol (20 ml) and acidified with ethanolic hydrogen chloride to afford the first diastereoisomer of the title compound as the trihydrochloride (227 mg), m.p. 140°-145° C. (Found: C,57.7;H,6.5;N,7.8 C26H31N3O3.3HCl requires C,57.5;H,6.3;N,7.7%).

후처리

  1. extractionextracted with dichloromethane (2×75 ml)
  2. extractionThe organic extract
  3. washwas washed (brine)
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customto give the first Rf diastereoisomer as a white foam which

출처 및 근거

ORD 기록
ord-f2564d9371f24ee9b7f9e11caa00f9fa
출처 데이터셋
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05346896

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