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5-[[3-(1,1-Dimethylethyl)-4-hydroxy-5-methylphenyl]methylene]-4-thiazolidinone → HCID 18936445, 화합물

HRID 2952
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반응식

HRID 2952 반응식
[CH3:1][C:2]([C:5]1[CH:6]=[C:7]([CH:13]=[C:14]2[S:18][CH2:17][NH:16][C:15]2=[O:19])[CH:8]=[C:9]([CH3:12])[C:10]=1[OH:11])([CH3:4])[CH3:3]>O1CCCC1.[Pd]>[CH3:4][C:2]([C:5]1[CH:6]=[C:7]([CH2:13][CH:14]2[S:18][CH2:17][NH:16][C:15]2=[O:19])[CH:8]=[C:9]([CH3:12])[C:10]=1[OH:11])([CH3:1])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 537701815-[[3-(1,1-Dimethylethyl)-4-hydroxy-5-methylphenyl]methylene]-4-thiazolidinone

생성물 1

HCID 18936445HCID 18936445, 화합물수율 17.7%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 0.28 g of the compound of Example 61 in 30 ml of tetrahydrofuran was hydrogenated at 60 pounds per square inch in the presence of 1.12 g of 5% palladium on carbon overnight at 60° C. The reaction mixture was filtered and evaporated to dryness. The resulting residue was dissolved in 3.5 ml of a 1:1.5 ethyl acetate/hexane solution and loaded onto a silica gel chromatography column. Elution with 40% ethyl acetate in hexane produced fractions which, upon evaporation to dryness, provided 0.05 g of title compound. m.p. 64°-68° C.

후처리

  1. filtrationThe reaction mixture was filtered
  2. customevaporated to dryness
  3. dissolutionThe resulting residue was dissolved in 3.5 ml of a 1:1.5 ethyl acetate/hexane solution
  4. washElution with 40% ethyl acetate in hexane produced fractions which
  5. customupon evaporation to dryness

출처 및 근거

ORD 기록
ord-4349083726d1496ca8ab1e9e85158d89
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05731336

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