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18-Crown-6 → HCID 14891674, 화합물

HRID 543562
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HRID 543562 반응식
[CH2:1]([CH:4]1[N:7]([Si](C(C)(C)C)(C)C)[C:6](=[O:15])[CH:5]1[CH3:16])[CH:2]=[CH2:3].[F-].[K+].C1OCCOCCOCCOCCOCCOC1>O1CCCC1>[CH2:1]([CH:4]1[NH:7][C:6](=[O:15])[CH:5]1[CH3:16])[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 2855718-Crown-6HCID 522689Potassium FluorideHCID 20461605HCID 20461605, 화합물

생성물 1

HCID 14891674HCID 14891674, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Part of the isomeric mixture from (ii) (1.20 g) in dry tetrahydrofuran (50 ml) was treated with potassium fluoride (0.45 g) and 18-crown-6 ether (0.07 g). After one hour the solution was partitioned between brine and ethylacetate. The organic phase was separated, dried (Na2SO4), evaporated and chromatographed on silica gel 60 (<230 mesh) eluting with ethylacetate:hexane 6:4. This separated the trans and cis isomers of 4-allyl-3-methyl azetidin-2-one.

후처리

  1. customAfter one hour the solution was partitioned between brine and ethylacetate
  2. customThe organic phase was separated
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customchromatographed on silica gel 60 (<230 mesh)
  6. washeluting with ethylacetate:hexane 6:4
  7. customThis separated the trans

출처 및 근거

ORD 기록
ord-9486123c9a724820aea2bc4bbe6823ab
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04446146

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