Hydrogen Sulfide → Methyl 1-methylpyrrol-2-acetate

HRID 1703752Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1703752
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7](=O)[C:8]([O:10][CH3:11])=[O:9].S>N1C=CC=CC=1>[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][C:8]([O:10][CH3:11])=[O:9]

Komponenten

4

Edukt 2

HCID 402Hydrogen Sulfide2×HCID 22759895Methyl 1-methyl-α-oxo-1H-pyrrole-2-acetate

Produkt 1

HCID 103992Methyl 1-methylpyrrol-2-acetateAusbeute 86 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Reaktionsbedingungen

Temperatur
63 °C

Versuchsvorschrift

A solution of 50g of methyl 1-methylpyrrole-2-glyoxylate in 200 ml of pyridine is cooled to -78° C. and 64g of hydrogen sulfide is added. The mixture is sealed in a stirred autoclave and heated to 63° C. The pressure rises to about 130 p.s.i. After 27 hrs., the hydrogen sulfide is driven off in a nitrogen stream and the solution is decanted from the precipitated sulfur. Pyridine is distilled off at 20 mm Hg. The residue is distilled at 0.03 mm Hg, b.p. 68-70° C., to give 39.2g of oily methyl 1-methylpyrrole-2-acetate (86% yield).

Aufarbeitung

  1. customThe mixture is sealed in a stirred autoclave
  2. customthe solution is decanted from the precipitated sulfur
  3. distillationPyridine is distilled off at 20 mm Hg
  4. distillationThe residue is distilled at 0.03 mm Hg, b.p. 68-70° C.

Quellen und Nachweise

ORD-Eintrag
ord-fc05f2eb207c43fca3530064e22b3743
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04125537

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