Ethyl Bromide → ST001145

HRID 1034338Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1034338
[CH3:1][C:2]1[NH:3][NH:4][C:5](=[O:7])[CH:6]=1.Br[CH2:9][CH3:10].C(=O)(O)[O-].[Na+]>>[CH2:9]([N:4]1[C:5](=[O:7])[CH2:6][C:2]([CH3:1])=[N:3]1)[CH3:10]

Komponenten

4

Edukt 3

HCID 6332Ethyl BromideHCID 3197713H-Pyrazol-3-one, 2,4-dihydro-5-methyl-HCID 516892Sodium Bicarbonate

Produkt 1

HCID 668049ST001145

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A mixture of 49 g 3-methyl-3-pyrazolin-5-one and 60.0 g bromoethane was sealed in a glass pressure tube and heated in an oil bath at 130° C. for 40 hours. After cooling, the tube was opened and the contents were poured into 200 g ice-water. Sodium bicarbonate (42.00 g) was added in small portions with stirring. The resulting mixture was stirred and heated to 100° C. for 1 hour, cooled to room temperature, and extracted with 10×50 ml portions of chloroform. The combined extracts were dried over anhydrous calcium chloride, evaporated under reduced pressure and the residue recrystallized from ethanol to give 20.1 g as colorless prisms, m.p. 112°-113° C.

Aufarbeitung

  1. customwas sealed in a glass pressure tube
  2. temperatureAfter cooling
  3. stirringThe resulting mixture was stirred
  4. temperatureheated to 100° C. for 1 hour
  5. temperaturecooled to room temperature
  6. extractionextracted with 10×50 ml portions of chloroform
  7. dry with materialThe combined extracts were dried over anhydrous calcium chloride
  8. customevaporated under reduced pressure
  9. customthe residue recrystallized from ethanol
  10. customto give 20.1 g as colorless prisms, m.p. 112°-113° C.

Quellen und Nachweise

ORD-Eintrag
ord-a5e9b92e3d764fd6a0d039aeaeb94ee1
Quelldatensatz
uspto-grants-1994_05
Patentnummer
US05314998

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