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Bromine → HCID 54404863, Verbindung

HRID 1758698
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1758698
C[CH:2]1C=C(C2C=CC=CC=2)[O:4][C:3]1=O.CC1C(=O)OC(C2C=CC=CC=2)C=1.[C:27]([CH2:35][CH:36]([CH3:49])[C:37]([N:39]1[CH:43]([C:44]([OH:46])=[O:45])[CH2:42][S:41][C:40]1([CH3:48])[CH3:47])=[O:38])(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.BrBr.C([O-])(=S)C.[K+]>C(O)(=O)C.C(O)(C)C.C(N(CC)CC)C>[C:3]([CH:35]([C:27](=[O:34])[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1)[CH:36]([CH3:49])[C:37]([N:39]1[C@H:43]([C:44]([OH:46])=[O:45])[CH2:42][S:41][C:40]1([CH3:48])[CH3:47])=[O:38])(=[O:4])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 24408BromineHCID 113557793-methyl-5-phenyl-2(5H)-furanoneHCID 131044283-Methyl-5-phenylfuran-2(3H)-oneHCID 23670855Potassium ethanethioateHCID 54245864HCID 54245864, Verbindung2×

Produkt 1

HCID 54404863HCID 54404863, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittelHCID 3776IsopropanolLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

A mixture of 8.39 g. (0.052 mole) of L-2,2-dimethylthiazolidine-4-carboxylic acid and 5.26 g. of triethylamine is heated on a steam bath. To the mixture is added 0.052 mole of a mixture of 3-methyl-5-phenyl-2(3H)-furanone and 3-methyl-5-phenyl-2(5H)-furanone in 150 ml. of dry isopropyl alcohol. The mixture is refluxed for 144 hours and the solvent is removed in vacuo. The residue is partitioned between water and ethyl acetate. The aqueous layer is poured onto crushed ice and acidified with hydrochloric acid. The mixture is extracted with ethyl acetate and the organic layer is dried over sodium sulfate. The solvent is removed to give 4.8 g. of a yellow glass which is a mixture of [4R-(4R*,2'R*)]-3-(3-benzoyl-2-methylpropionyl)-2,2-dimethyl-4-thiazolidinecarboxylic acid and [4R-(4R*,2'S*)]-3-(3-benzoyl-2-methylpropionyl)-2,2-dimethyl-4-thiazolidinecarboxylic acid. The mixture is dissolved in acetic acid containing anhydrous hydrogen bromide gas and to the mixture is added bromine. Removal of the solvent gives a glass which is reacted with potassium thioacetate as in the procedure of Example 1 to give the product of the Example as a mixture of diastereomers.

Aufarbeitung

  1. additionA mixture of 8.39 g
  2. temperatureThe mixture is refluxed for 144 hours
  3. customthe solvent is removed in vacuo
  4. customThe residue is partitioned between water and ethyl acetate
  5. additionThe aqueous layer is poured
  6. customonto crushed ice
  7. extractionThe mixture is extracted with ethyl acetate
  8. dry with materialthe organic layer is dried over sodium sulfate
  9. customThe solvent is removed
  10. customto give 4.8 g
  11. customRemoval of the solvent
  12. customgives a glass which
  13. customto give the product of the Example
  14. additionas a mixture of diastereomers

Quellen und Nachweise

ORD-Eintrag
ord-12c3bd6fb8c745c399fedbc21d47396d
Quelldatensatz
uspto-grants-1983_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04374249

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