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Pyridine → HCID 11145881, Verbindung

HRID 1249588
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1249588
N1C=CC=CC=1.CN(C)C=O.S(Cl)([Cl:14])=O.O[CH2:17][C:18]1[CH2:19][S:20][C@@H:21]2[C@H:41]([NH:42][C:43](=[O:51])[CH2:44][C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=3)[C:40](=[O:52])[N:22]2[C:23]=1[C:24]([O:26][CH:27]([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:25]>O1CCCC1>[Cl:14][CH2:17][C:18]1[CH2:19][S:20][C@@H:21]2[C@H:41]([NH:42][C:43](=[O:51])[CH2:44][C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=3)[C:40](=[O:52])[N:22]2[C:23]=1[C:24]([O:26][CH:27]([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:25]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 1049PyridineHCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 10864182HCID 10864182, Verbindung

Produkt 1

HCID 11145881HCID 11145881, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028
Tetrahydrofuran
Lösungsmittel

Versuchsvorschrift

24 ml (0.3 mol) of pyridine, 400 μl of dimethylformamide and 21.6 ml (0.3 mol) of thionyl chloride are added, while cooling in ice, to a solution of 103 g (0.2 mol) of benzhydryl 3-hydroxymethyl-7β-phenylacetamido-3-cephem-4-carboxylate (prepared according to, for example, Helv. Chim. Acta 57, 2044 (1974)) in 3.5 l of absolute tetrahydrofuran. After 10 minutes, the mixture is evaporated in a rotary evaporator, the residue is taken up in 2 l of ethyl acetate, and the solution is extracted by shaking twice with sodium bicarbonate solution and once with water. The organic phase is stirred with 50 g each of kieselguhr and active charcoal and filtered with suction through a sintered glass funnel containing silica gel. It is then dried over magnesium sulphate, evaporated, and residue is taken up in 200 ml of methylene chloride and the product is precipitated with petroleum ether.

Aufarbeitung

  1. customthe mixture is evaporated in a rotary evaporator
  2. extractionthe solution is extracted
  3. stirringThe organic phase is stirred with 50 g each of kieselguhr and active charcoal
  4. filtrationfiltered with suction through a sintered glass funnel
  5. additioncontaining silica gel
  6. dry with materialIt is then dried over magnesium sulphate
  7. customevaporated
  8. customthe product is precipitated with petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-3a464bbf7add4a74b8104afc0f24575b
Quelldatensatz
uspto-grants-1986_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04632918

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