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Water → 5-[4-(5-Methyl-2-phenyl-4-oxazolylmethoxy)benzylidene]-2,4-thiazolidinedione

HRID 4393
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인쇄 미리보기

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HRID 4393 반응식
[H-].[Na+].[OH:3][C:4]1[CH:17]=[CH:16][C:7]([CH:8]=[C:9]2[S:13][C:12](=[O:14])[NH:11][C:10]2=[O:15])=[CH:6][CH:5]=1.Cl[CH2:19][C:20]1[N:21]=[C:22]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[O:23][C:24]=1[CH3:25].O>CN(C)C=O.C(O)(=O)C>[CH3:25][C:24]1[O:23][C:22]([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)=[N:21][C:20]=1[CH2:19][O:3][C:4]1[CH:17]=[CH:16][C:7]([CH:8]=[C:9]2[S:13][C:12](=[O:14])[NH:11][C:10]2=[O:15])=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 5178225-((4-Hydroxyphenyl)methylene)-2,4-thiazolidinedioneHCID 97942894-(Chloromethyl)-5-methyl-2-phenyl-1,3-oxazole

생성물 1

HCID 542390285-[4-(5-Methyl-2-phenyl-4-oxazolylmethoxy)benzylidene]-2,4-thiazolidinedione수율 41.6%

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 6228Dimethylformamide용매2회

실험 절차

60% sodium hydride in oil (0.24 g) was added to a solution of 5-(4-hydroxybenzylidene)-2,4-thiazolidinedione (0.664 g) in N,N-dimethylformamide (20 ml), and the mixture was stirred for 30 minutes. A solution of 4-chloromethyl-5-methyl-2-phenyloxazole (0.623 g) in N,N-dimethylformamide (10 ml) was added dropwise to the mixture under ice-cooling. After stirring at room temperature for 5 hours, the reaction solution was poured into water. The aqueous mixture was made acid with acetic acid and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4) and concentrated. The residue was chromatographed on a column of silica gel (50 g). From the fractions eluted with ethyl acetatehexane (1:2, V/V), there was obtained 5-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzylidene]-2,4-thiazolidinedione (0.49 g, 40.8%). Recrystallization from chloroform-methanol afforded colorless prisms, m.p. 225°-226° C. Elemental analysis for C21H16N2O4S, Calcd.: C, 64.27; H, 4.11; N, 7.14. Found: C, 64.49; H, 3.96; H, 6.86.

후처리

  1. temperaturecooling
  2. stirringAfter stirring at room temperature for 5 hours
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with water
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customThe residue was chromatographed on a column of silica gel (50 g)
  8. washFrom the fractions eluted with ethyl acetatehexane (1:2, V/V)

출처 및 근거

ORD 기록
ord-59eb3a84c5114e449b61d0353ae198d1
출처 데이터셋
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04725610

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