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2-Methyl-2-butene → HCID 67474068, Verbindung

HRID 2387751
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2387751
CC(=CC)C.P([O-])(O)(O)=O.[Na+].Cl([O-])=[O:13].[Na+].[F:16][C:17]1[CH:18]=[C:19]([C@:23]2([CH2:28][O:29][C:30]3[C:35](=[O:36])[N:34]([CH2:37][O:38][CH3:39])[C:33]([CH3:40])=[N:32][C:31]=3[CH3:41])[CH2:25][C@H:24]2[CH:26]=[O:27])[CH:20]=[CH:21][CH:22]=1>C(Cl)(Cl)Cl.O.CC(C)=O.O>[F:16][C:17]1[CH:18]=[C:19]([C@:23]2([CH2:28][O:29][C:30]3[C:35](=[O:36])[N:34]([CH2:37][O:38][CH3:39])[C:33]([CH3:40])=[N:32][C:31]=3[CH3:41])[CH2:25][C@H:24]2[C:26]([OH:13])=[O:27])[CH:20]=[CH:21][CH:22]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 105532-Methyl-2-buteneHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphateHCID 87337461HCID 87337461, Verbindung

Produkt 1

HCID 67474068HCID 67474068, VerbindungAusbeute 100,1 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962
Water
Lösungsmittel
HCID 6212ChloroformLösungsmittel
HCID 18366337Propan-2-one--water (1/1)Lösungsmittel

Versuchsvorschrift

2-methyl 2-butene (1.14 ml), sodium dihydrogen phosphate (389 mg) and sodium chlorite (305 mg) were added to an acetone-water mixed solvent (8 ml-2 ml) of the compound 326-8 (779 mg). The obtained mixture was stirred at room temperature for 1 hour. Thereafter, water was added to the reaction solution, and chloroform was added to the reaction solution to carry out liquid separation and extraction. A small amount of 1 N hydrochloric acid was added to the obtained extract, and chloroform was further added to the reaction solution to carry out liquid separation and extraction. The obtained organic layer was dried over magnesium sulfate. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, so as to obtain a crude product of the title carboxylic acid (814 mg).

Aufarbeitung

  1. additionwas added to the reaction solution
  2. customliquid separation and extraction
  3. additionA small amount of 1 N hydrochloric acid was added to the obtained
  4. extractionextract
  5. additionchloroform was further added to the reaction solution
  6. customliquid separation and extraction
  7. dry with materialThe obtained organic layer was dried over magnesium sulfate
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-19b186198e2a453a97bcd384826e235e
Quelldatensatz
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08268848B2

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