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3-Pyridinemethanol → HCID 53682346, 화합물

HRID 1200056
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HRID 1200056 반응식
[S:1]1[CH:5]=[C:4]([CH:6]=[CH:7][C:8]2[S:12][C:11]([C:13](Cl)=[O:14])=[CH:10][CH:9]=2)[C:3]2[CH:16]=[CH:17][CH:18]=[CH:19][C:2]1=2.N1C=CC=C(C[OH:27])C=1>N1C=CC=CC=1>[S:1]1[CH:5]=[C:4]([CH:6]=[CH:7][C:8]2[S:12][C:11]([C:13]([OH:27])=[O:14])=[CH:10][CH:9]=2)[C:3]2[CH:16]=[CH:17][CH:18]=[CH:19][C:2]1=2
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참가 물질

4

반응물 2

HCID 75103-PyridinemethanolHCID 539913705-[2-(Benzo[b]thiophen-3-yl)ethenyl]thiophene-2-carboxylic acid chloride

생성물 1

HCID 53682346HCID 53682346, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

The acid chloride of 5-[2-(benzo[b]thiophen-3-yl)ethenyl]thiophene-2-carboxylic acid was prepared as described in Example 9. To a suspension of 5-[2-(benzo[b]thiophen-3-yl)ethenyl]thiophene2-carboxylic acid chloride (5.00 g) and pyridine (50 ml) was added 3-pyridylcarbinol (1.79 g). After refluxing overnight, the mixture was evaporated, and the residue was dissolved in ether, filtered, and concentrated. The residue was purified by high performance liquid chromatography (silica gel, eluted with 2:1 ethyl acetate:hexane). The appropriate fractions were combined and evaporated. The residue was recrystallized from toluene/hexane to afford 1.4 g (23%) of the product, mp 97°-98° C.

후처리

  1. temperatureAfter refluxing overnight
  2. customthe mixture was evaporated
  3. dissolutionthe residue was dissolved in ether
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by high performance liquid chromatography (silica gel, eluted with 2:1 ethyl acetate:hexane)
  7. customevaporated
  8. customThe residue was recrystallized from toluene/hexane

출처 및 근거

ORD 기록
ord-1592a9c9c70a4632af2721e3e6f41298
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04904674

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