Hydrazine, acetate (1:1) → HCID 68863971, Verbindung

HRID 494124Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 494124
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]2[C:8]([C:18](=O)[C:19]([O:21][CH3:22])=[O:20])=[C:9]([C:13](OCC)=[O:14])[C:10]([O:11][CH3:12])=[C:4]2[C:3]1=[O:24].C(OC(NCC(N(CC(OC)OC)C)=O)=O)C1C=CC=CC=1.C(O)(=O)C.[NH2:51][NH2:52]>C(O)(=O)C>[CH3:12][O:11][C:10]1[C:9]2[C:13](=[O:14])[NH:52][N:51]=[C:18]([C:19]([O:21][CH3:22])=[O:20])[C:8]=2[N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[C:3](=[O:24])[C:4]=12

Komponenten

5

Edukt 3

HCID 165591Hydrazine, acetate (1:1)HCID 58009747HCID 58009747, VerbindungHCID 68865401HCID 68865401, Verbindung

Produkt 1

HCID 68863971HCID 68863971, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

A solution of ethyl 2-methyl-8-(methoxy)-6-[methoxy(oxo)acetyl]-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine-7-carboxylate (1.28 g, 3.78 mmol; prepared in a manner similar to that described in Example 62, step 5 to 8, starting with 1-methylpiperazin-2-one (Example 7, step 1 to 3) and hydrazine acetate (1.05 g, 11.36 mmol) in glacial acetic acid (8 mL) was heated at 160° C. in an microwave oven for 20 minutes. The mixture was concentrated under vacuum. The residue was partitioned between chloroform and brine. The organic extract was dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residue was triturated in a 4:1 mixture of ethanol and diethyl ether. The precipitate was filtered to afford the title compound. ES MS M+1=321

Aufarbeitung

  1. customprepared in a manner similar to
  2. concentrationThe mixture was concentrated under vacuum
  3. customThe residue was partitioned between chloroform and brine
  4. extractionThe organic extract
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum
  8. customThe residue was triturated in a 4:1 mixture of ethanol and diethyl ether
  9. filtrationThe precipitate was filtered

Quellen und Nachweise

ORD-Eintrag
ord-91fb736e81e641519cdf14ef56ffe676
Quelldatensatz
uspto-grants-2009_05
Patentnummer
US07538112B2

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