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Water → 5-{4-[2-(1-Methylcyclohexyl)-4-oxazolylmethoxy]benzyl}-2,4-thiazolidinedione

HRID 4387
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 4387
[H-].[Na+].[OH:3][C:4]1[CH:17]=[CH:16][C:7]([CH2:8][CH: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:25]2([CH3:31])[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]2)[O:23][CH:24]=1.O>CN(C)C=O>[CH3:31][C:25]1([C:22]2[O:23][CH:24]=[C:20]([CH2:19][O:3][C:4]3[CH:17]=[CH:16][C:7]([CH2:8][CH:9]4[S:13][C:12](=[O:14])[NH:11][C:10]4=[O:15])=[CH:6][CH:5]=3)[N:21]=2)[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 24758Sodium hydrideHCID 101983975-(4-Hydroxybenzyl)thiazolidine-2,4-dioneHCID 201524064-Chloromethyl-2-(1-methylcyclohexyl)oxazole

Produkt 1

HCID 137139035-{4-[2-(1-Methylcyclohexyl)-4-oxazolylmethoxy]benzyl}-2,4-thiazolidinedione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel
2×

Versuchsvorschrift

60% sodium hydride in oil (1.32 g) was added to solution of 5-(4-hydroxybenzyl)-2,4-thiazolidinedione (3.35 g) in N,N-dimethylformamide (30 ml), and the mixture was stirred for 30 minutes. Then, solution of 4-chloromethyl-2-(1-methylcyclohexyl)oxazole (3.85 g) in N,N-dimethylformamide (5 ml) was added dropwise thereto at room temperature. After being stirred at 60° C. for 1 hour, the reaction solution was poured into water, and the aqueous mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4) and concentrated. The oily residue was chromatographed on a column of silica gel (70 g). Elution with hexaneethyl acetate (2:1, V/V) gave 5-{4-[2-(1-methylcyclohexyl)-4-oxazolylmethoxy]benzyl}-2,4-thiazolidinedione as an oily substance. A solution of sodium 2-ethylhexanoate in isopropanol (2N, 3 ml) was added to the oily substance, and treated with ether. The crystals which separated out were collected by filtration to give 5- {4-[2-(1-methylcyclohexyl)-4-oxazolylmethoxy]benzyl}-2,4-thiazolidinedione.sodium salt (2.3 g, 36.3%). Recrystallization from methanol afforded colorless plates. m.p. 285°-287° C. (decomp.) Elemental analysis for C21H23N2O4SNa, Calcd.: C, 59.70; H, 5.49; N, 6.63. Found: C, 59.76; H, 5.56; N, 6.82.

Aufarbeitung

  1. customat room temperature
  2. stirringAfter being stirred at 60° C. for 1 hour
  3. extractionthe aqueous mixture was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with water
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customThe oily residue was chromatographed on a column of silica gel (70 g)
  8. washElution with hexaneethyl acetate (2:1, V/V)

Quellen und Nachweise

ORD-Eintrag
ord-1600130bf31e4d3497fdf571ee839211
Quelldatensatz
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04725610

Notizen zur Reaktion

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