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Hydrochloric Acid → methyl (2E)-3-(4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]vinyl}thiophen-2-yl)acrylate

HRID 1892507
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1892507
[Cl-].[C:2]([NH:5][C:6]1[S:7][CH:8]=[C:9]([CH2:11][P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[N:10]=1)(=[O:4])[CH3:3].CC(C)([O-])C.[K+].[CH:37]([C:39]1[CH:40]=[C:41](/[CH:44]=[CH:45]/[C:46]([O:48][CH3:49])=[O:47])[S:42][CH:43]=1)=O.Cl.[Cl-].[Na+]>CN(C)C=O>[C:2]([NH:5][C:6]1[S:7][CH:8]=[C:9]([CH:11]=[CH:37][C:39]2[CH:40]=[C:41](/[CH:44]=[CH:45]/[C:46]([O:48][CH3:49])=[O:47])[S:42][CH:43]=2)[N:10]=1)(=[O:4])[CH3:3]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 23665647Potassium tert-butoxideHCID 86092822[(2-Acetylaminothiazol-4-yl)methyl](triphenyl)phosphonium chlorideHCID 86650009methyl (2E)-3-(4-formylthiophen-2-yl)acrylate

Produkt 1

HCID 86650010
methyl (2E)-3-(4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]vinyl}thiophen-2-yl)acrylate
Ausbeute 82,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To {[2-(acetylamino)-1,3-thiazol-4-yl]methyl}(triphenyl)phosphoniumchloride (6.602 g, 14.58 mmol) was added anhydrous N,N-dimethylformamide (30 ml), and the mixture was cooled to 0° C. Potassium tert-butoxide (3.146 g, 28.03 mmol) was added, and the mixture was stirred at 0° C. for 15 min. A solution of methyl (2E)-3-(4-formylthiophen-2-yl)acrylate (2.200 g, 11.21 mmol) in anhydrous N,N-dimethylformamide (30 ml) was added dropwise, and the mixture was stirred at 0° C. for 1 hr. The reaction mixture was poured into ice-cooled dil. hydrochloric acid (600 ml, containing 15 mmol as HCl). Sodium chloride (10 g) was added, and the mixture was extracted 3 times with ethyl acetate. The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (FUJI SILYSIA CHEMICAL LTD. BW-300SP 500 g, ethyl acetate:hexane=1:1) to give methyl (2E)-3-(4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]vinyl}thiophen-2-yl)acrylate (3.090 g, 9.241 mmol, 82.4%) as a yellowish-white solid.

Aufarbeitung

  1. stirringthe mixture was stirred at 0° C. for 1 hr
  2. additionThe reaction mixture was poured into ice-
  3. extractionthe mixture was extracted 3 times with ethyl acetate
  4. washThe combined organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (FUJI SILYSIA CHEMICAL LTD. BW-300SP 500 g, ethyl acetate:hexane=1:1)

Quellen und Nachweise

ORD-Eintrag
ord-4fe7580cdc7640609dcd1f89699e5378
Quelldatensatz
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08507690B2

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