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1,3-Bis(trimethylsilyl)urea → benzhydryl (6R,7R)-7-[[(2Z)-2-acetyloxyimino-2-(2-amino-1,3-thiazol-4-yl)acetyl]amino]-8-oxo-3-(1H-pyrazol-4-ylmethylsulfanyl)-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate

HRID 992707
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 992707
[NH2:1][C@@H:2]1[C:32](=[O:33])[N:4]2[C:5]([C:16]([O:18][CH:19]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:17])=[C:6]([S:9][CH2:10][C:11]3[CH:12]=[N:13][NH:14][CH:15]=3)[CH2:7][S:8][C@H:3]12.C[Si](C)(C)NC(N[Si](C)(C)C)=O.[NH2:46][C:47]1[S:48][CH:49]=[C:50](/[C:52](=[N:56]/[O:57][C:58](=[O:60])[CH3:59])/[C:53](Cl)=[O:54])[N:51]=1.C(=O)(O)[O-].[Na+]>C1COCC1.C(#N)C.C(OCC)(=O)C>[NH2:46][C:47]1[S:48][CH:49]=[C:50](/[C:52](=[N:56]/[O:57][C:58](=[O:60])[CH3:59])/[C:53]([NH:1][C@@H:2]2[C:32](=[O:33])[N:4]3[C:5]([C:16]([O:18][CH:19]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)[C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=4)=[O:17])=[C:6]([S:9][CH2:10][C:11]4[CH:15]=[N:14][NH:13][CH:12]=4)[CH2:7][S:8][C@H:3]23)=[O:54])[N:51]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 875621,3-Bis(trimethylsilyl)ureaHCID 516892Sodium BicarbonateHCID 11322595[(Z)-[1-(2-amino-1,3-thiazol-4-yl)-2-chloro-2-oxoethylidene]amino] acetateHCID 70122266Diphenylmethyl 7beta-amino-3-[(pyrazol-4-yl)methylthio]-3-cephem-4-carboxylate

Produkt 1

HCID 88158439
benzhydryl (6R,7R)-7-[[(2Z)-2-acetyloxyimino-2-(2-amino-1,3-thiazol-4-yl)acetyl]amino]-8-oxo-3-(1H-pyrazol-4-ylmethylsulfanyl)-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6342AcetonitrileLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
35 °C

Versuchsvorschrift

Under nitrogen atmosphere, to a suspension of diphenylmethyl 7β-amino-3-[(pyrazol-4-yl)methylthio]-3-cephem-4-carboxylate (30.2 g) in THF (800 ml) was added herein 1,3-bis(trimethylsilyl)urea (25.8 g) was added at the room temperature. The reaction mixture was warmed at 35° C. and dissolved, and then it was cooled below 0° C. A suspension of 2-(2-aminothiazol-4-yl)-2-(Z)-(acetoxyimino)acetylchloride monohydrochiloride salt (17.93 g) in acetonitrile (200 ml) was dropped into the above reaction mixture below 0° C. After stirring at the same temperature for 10 minutes, it was poured into a mixture of ethyl acetate (1.2 l) and ice-water (1.5 l). The aqueous layer was adjusted at pH 6.5 with saturated sodium bicarbonate solution. The organic layer was separated, washed with brine (1.0 l), and dried over magnesium sulfate, and then evaporated until the volume amounted to 500 ml. The solution was poured into IPE (1.5 l). The resulting precipitate was filtered, dried under reduced pressure to give diphenylmethyl 7β-[2-(2-aminothiazol-4-yl)-2-(Z)-(acetoxyimino)acetamido]-3-[(pyrazol-4-yl)methylthio]-3-cephem-4-carboxylate (41.3 g) as powder.

Aufarbeitung

  1. additionwas added at the room temperature
  2. dissolutiondissolved
  3. temperatureit was cooled below 0° C
  4. additionwas dropped into the above reaction mixture below 0° C
  5. customThe organic layer was separated
  6. washwashed with brine (1.0 l)
  7. dry with materialdried over magnesium sulfate
  8. customevaporated until the volume
  9. additionThe solution was poured into IPE (1.5 l)
  10. filtrationThe resulting precipitate was filtered
  11. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b7c71077da35489a8f8cb2c4e1afde81
Quelldatensatz
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06468995B1

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