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Lithium hydroxide, monohydrate → HCID 9935937, Verbindung

HRID 2305341
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2305341
C[O:2][C:3]([C:5]1[N:6]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[C:33]([F:36])([F:35])[F:34])[S:7](=[O:26])(=[O:25])[C:8]2[CH:24]=[CH:23][CH:22]=[CH:21][C:9]=2[C:10]=1[C:11]1[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[CH:12]=1)=[O:4].O.[OH-].[Li+]>CO.O>[CH3:18][O:17][C:15]1[CH:16]=[C:11]([C:10]2[C:9]3[CH:21]=[CH:22][CH:23]=[CH:24][C:8]=3[S:7](=[O:26])(=[O:25])[N:6]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[C:33]([F:36])([F:34])[F:35])[C:5]=2[C:3]([OH:4])=[O:2])[CH:12]=[C:13]([O:19][CH3:20])[CH:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 15512895HCID 15512895, Verbindung

Produkt 1

HCID 9935937HCID 9935937, VerbindungAusbeute 66 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

The solution of 4-(3,5-dimethoxy-phenyl)-2-(2-trifluoromethyl-phenyl)-1,1-dioxo-1,2-dihydro-1λ6-benzo[e][1,2]thiazine-3-carboxylic acid methyl ester (1.29 g, 2.5 mmol) and lithium hydroxide monohydrate (0.3 g 12.5 mmol) in 30 mL of MeOH and 15 mL water was refluxed for 2.5 hours and evaporated to an oil. The residue was dissolved in water, washed with ethyl ether, and the aqueous layer decanted. The aqueous layer was acidified to pH 1 with concentrated HCl and extracted into ethyl ether, washed with brine, dried over anhydrous magnesium sulfate, filtered, and evaporated to a foam. The residue was chromatographed on 50 g silica gel eluted with chloroform, and the appropriate fractions were concentrated in vacuo and evaporated from ethyl ether giving a solid foam, 1.4 g, 66% yield. NMR spectra and elemental analysis were consistent with the structure.

Aufarbeitung

  1. customevaporated to an oil
  2. dissolutionThe residue was dissolved in water
  3. washwashed with ethyl ether
  4. customthe aqueous layer decanted
  5. extractionextracted into ethyl ether
  6. washwashed with brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customevaporated to a foam
  10. customThe residue was chromatographed on 50 g silica gel
  11. washeluted with chloroform
  12. concentrationthe appropriate fractions were concentrated in vacuo
  13. customevaporated from ethyl ether giving a solid foam, 1.4 g, 66% yield

Quellen und Nachweise

ORD-Eintrag
ord-b38cf03987d74a5897cbbf5dde141b18
Quelldatensatz
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06440962B2

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