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Solketal → HCID 53682346, 화합물

HRID 1200054
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HRID 1200054 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.CC1(C)OC(CO)C[O:22]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:22])=[O:14])=[CH:10][CH:9]=2)[C:3]2[CH:16]=[CH:17][CH:18]=[CH:19][C:2]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7528SolketalHCID 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 solution of 5-[2-(benzo[b]thiophen-3-yl)ethenyl]thiophene-2-carboxylic acid chloride (5.0 g) and pyridine (50 ml) was added 2,2-dimethyl-1,3-dioxolane-4-methanol (2.17 g). After refluxing overnight, the mixture was evaporated. The residue was dissolved in ethyl acetate, filtered, and concentrated. The residue was purified by high performance liquid chromatography (silica gel, loaded and eluted in 2:1 ethyl acetate:hexane). The appropriate fractions were combined and evaporated. Trituration of the residue with hexane yielded 2.60 g (39%) of product, mp 77°-79° C.

후처리

  1. temperatureAfter refluxing overnight
  2. customthe mixture was evaporated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by high performance liquid chromatography (silica gel, loaded and eluted in 2:1 ethyl acetate:hexane)
  7. customevaporated

출처 및 근거

ORD 기록
ord-23c7f285a13a4ca1b52e29e9185b8772
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04904674

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