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Ethyl Acetate → [2-(4-Methoxyphenyl)-6-methoxybenzo[b]thien-3-yl][2-[2-(1-piperidinyl)ethoxy]pyridin-5-yl]methanone

HRID 2293959
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HRID 2293959 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:13][C:12]3[CH:14]=[C:15]([O:18][CH3:19])[CH:16]=[CH:17][C:11]=3[C:10]=2[C:20]([C:22]2[CH:23]=[CH:24][C:25](Cl)=[N:26][CH:27]=2)=[O:21])=[CH:5][CH:4]=1.[Na].CCO[C:33]([CH3:35])=[O:34]>C1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:13][C:12]3[CH:14]=[C:15]([O:18][CH3:19])[CH:16]=[CH:17][C:11]=3[C:10]=2[C:20]([C:22]2[CH:23]=[CH:24][C:25]([O:34][CH2:33][CH2:35][N:26]3[CH2:27][CH2:22][CH2:23][CH2:24][CH2:25]3)=[N:26][CH:27]=2)=[O:21])=[CH:5][CH:4]=1
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참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 5360545Sodium2회HCID 23512898(6-Chloro-pyridin-3-yl)-[6-methoxy-2-(4-methoxy-phenyl)-benzo[b]thiophen-3-yl]-methanone

생성물 1

HCID 12992504[2-(4-Methoxyphenyl)-6-methoxybenzo[b]thien-3-yl][2-[2-(1-piperidinyl)ethoxy]pyridin-5-yl]methanone

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
70 °C

실험 절차

[2-(4-Methoxyphenyl)-6-methoxybenzo[b]thien-3-yl][2-chloropyridin-5-yl]methanone (1 g, 2.44 mmol) was dissolved in 10 mL of benzene and 950 mg (7.32 mmol) of 2-hydroxyethyl-1-piperidine was added. To the reaction mixture was added 85 mg (3.7 mmol) of sodium and the reaction was stirred at ambient temperature under a nitrogen atmosphere until all the sodium dissolved. The reaction was heated to 70° C. for two and half hours, then allowed to cool. To the reaction solution was added 150 mL of EtOAc and the solution was washed three times with saturated aqueous Na2CO3. The organic layer was separated and evaporated to dryness. The crude product was chromatographed on a silica gel column eluted with a linear gradient beginning with CHCl3 and ending with CHCl3 -MeOH (19:1). The desired fraction were determined by tlc, combined, and evaporated to dryness. This yielded the title compound as a yellow, amorphous solid.

후처리

  1. dissolutiondissolved
  2. temperatureto cool
  3. washthe solution was washed three times with saturated aqueous Na2CO3
  4. customThe organic layer was separated
  5. customevaporated to dryness
  6. customThe crude product was chromatographed on a silica gel column
  7. washeluted with a linear gradient
  8. customevaporated to dryness

출처 및 근거

ORD 기록
ord-164baf96c3c04b2d87520d17505eac42
출처 데이터셋
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05688796

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