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Oxalic Acid → HCID 178441403, Verbindung

HRID 2231434
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2231434
C(=O)([O-])[O-].[Ba+2].[C:6]([OH:11])(=[O:10])[C:7]([OH:9])=[O:8].[CH3:12][CH2:13][CH2:14][CH2:15][CH:16]1[C:51](=[O:52])[O:50][CH:49]([CH:53]([CH:55]([OH:63])[CH2:56][CH2:57][CH2:58][NH:59][C:60]([NH2:62])=[NH:61])[CH3:54])[CH:48]([CH3:64])[CH:47]=[C:46]([CH3:65])[CH2:45][CH2:44][CH2:43][CH2:42][CH:41]([OH:66])[CH2:40][CH:39]([OH:67])[CH2:38][CH:37]([OH:68])[CH2:36][CH:35]([OH:69])[CH2:34][CH:33]([OH:70])[CH:32]([O:71][C@H:72]2[O:76][C@H:75]([CH2:77][OH:78])[C@@H:74]([OH:79])[C@@H:73]2[OH:80])[CH:31]=[C:30]([CH3:81])[CH:29]([OH:82])[CH2:28][CH2:27][CH2:26][CH:25]([OH:83])[CH2:24][CH2:23][CH2:22][CH:21]([OH:84])[CH2:20][CH2:19][CH:18]([CH3:85])[CH:17]1[OH:86].S([O-])([O-])(=O)=O>CO>[CH3:12][CH2:13][CH2:14][CH2:15][CH:16]1[C:51](=[O:52])[O:50][CH:49]([CH:53]([CH:55]([OH:63])[CH2:56][CH2:57][CH2:58][NH:59][C:60]([NH2:62])=[NH:61])[CH3:54])[CH:48]([CH3:64])[CH:47]=[C:46]([CH3:65])[CH2:45][CH2:44][CH2:43][CH2:42][CH:41]([OH:66])[CH2:40][CH:39]([OH:67])[CH2:38][CH:37]([OH:68])[CH2:36][CH:35]([OH:69])[CH2:34][CH:33]([OH:70])[CH:32]([O:71][C@H:72]2[O:76][C@H:75]([CH2:77][OH:78])[C@@H:74]([OH:79])[C@@H:73]2[OH:80])[CH:31]=[C:30]([CH3:81])[CH:29]([OH:82])[CH2:28][CH2:27][CH2:26][CH:25]([OH:83])[CH2:24][CH2:23][CH2:22][CH:21]([OH:84])[CH2:20][CH2:19][CH:18]([CH3:85])[CH:17]1[OH:86].[C:6]([O-:11])(=[O:10])[C:7]([O-:9])=[O:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 971Oxalic AcidHCID 10563Barium CarbonateHCID 178441404HCID 178441404, Verbindung

Produkt 1

HCID 178441403HCID 178441403, VerbindungAusbeute 179,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

0.087 g (0.444 millimoles) of barium carbonate are suspended in 15 ml of mthanol whereupon 0.04 g (0.444 millimoles) of oxalic acid are added. The suspension thus obtained is heated to boiling until all the solid is dissolved (about 10 minutes). The solvent is removed in vacuo. The residue is added to a solution of 1.0 g (0.887 millimoles) of primycin sulfate and 80 ml of methanol and the reaction mixture is heated to boiling for 20 minutes under constant stirring. The precipitated barium sulfate is filtered hot over Celite. The filtrate is evaporated in vacuo. The solid residue is treated with ether and filtered. The solid is washed on the filter with a 2:1 mixture of acetone and water. Thus 0.93 g of white primycin oxalate is obtained, yield 92.2%. Mp.: 186°-187° C., /α/D25 =+40°.

Aufarbeitung

  1. additionare added
  2. customThe suspension thus obtained
  3. temperatureis heated
  4. dissolutionis dissolved (about 10 minutes)
  5. customThe solvent is removed in vacuo
  6. temperaturethe reaction mixture is heated
  7. filtrationThe precipitated barium sulfate is filtered hot over Celite
  8. customThe filtrate is evaporated in vacuo
  9. additionThe solid residue is treated with ether
  10. filtrationfiltered
  11. washThe solid is washed on the
  12. filtrationfilter with a 2:1 mixture of acetone and water

Quellen und Nachweise

ORD-Eintrag
ord-8a943763963d446bb305abcf60f45e8d
Quelldatensatz
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04782141

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