Formaldehyde → Ranisen

HRID 65762

Reaktionsgleichung

Reaktionsgleichung von HRID 65762
[CH3:1][N:2]([CH3:9])[CH2:3][C:4]1[O:5][CH:6]=[CH:7][CH:8]=1.[CH2:10]=O.[SH:12][CH2:13][CH2:14][NH:15][C:16]([NH:21][CH3:22])=[CH:17][N+:18]([O-:20])=[O:19]>C(O)(=O)C.Cl.O.C(=O)([O-])[O-].[K+].[K+]>[CH3:1][N:2]([CH2:3][C:4]1[O:5][C:6]([CH2:10][S:12][CH2:13][CH2:14][NH:15][C:16]([NH:21][CH3:22])=[CH:17][N+:18]([O-:20])=[O:19])=[CH:7][CH:8]=1)[CH3:9]

Komponenten

8

Edukt 3

HCID 712FormaldehydeHCID 84478N,N-dimethyl-2-FuranmethanamineHCID 181798N-(2-Mercaptoethyl)-N'-methyl-2-nitro-1,1-ethenediamine

Produkt 1

HCID 5039Ranisen

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 176Acetic AcidLösungsmittel2×HCID 313Hydrochloric AcidLösungsmittelHCID 962WaterLösungsmittelHCID 11430Potassium CarbonateLösungsmittel

Versuchsvorschrift

N,N-Dimethyl-2-furanmethanamine (125 mg) was dissolved in glacial acetic acid (1 ml) and paraformaldehyde (30 mg) added. A solution of N-(2-mercaptoethyl)-N'-methyl-2-nitro-1,1-ethenediamine (354 mg) in concentrated hydrochloric acid (1 ml) and glacial acetic acid (1 ml) was added dropwise and the mixture left to stand at room temperature for 5 days. The solution was diluted with water (30 ml), saturated with potassium carbonate and extracted with ethyl acetate. The combined extracts were purified by preparative layer chromatography to give the title compound as Example 15 (89 mg).

Aufarbeitung

  1. waitthe mixture left
  2. extractionextracted with ethyl acetate
  3. customThe combined extracts were purified by preparative layer chromatography

Quellen und Nachweise

ORD-Eintrag
ord-96c1dc2b93d34428a79bb765cbb242c8
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04128658

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