Reaktion #522987

ord-68289026b5b44592bd76e0767cbb162a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe aqueous mixture extracted with diethyl ether
  2. 2
    ExtraktionThe ether extract
  3. 3
    Waschenwas washed
  4. 4
    workup.ADDITIONwith dilute acid
  5. 5
    Trocknenwith water and with saturated sodium chloride solution and dried
  6. 6
    SonstigeEvaporation of the ether

Vorschrift

A mixture of 6.6 g of carbofuran and 4.8 g of morpholinosulfenyl chloride in 40 ml of pyridine was allowed to stand at room temperature for about 18 hours. The mixture, which contained solid pyridine hydrochloride, was poured into water and the aqueous mixture extracted with diethyl ether. The ether extract was washed with dilute acid, then with water and with saturated sodium chloride solution and dried. Evaporation of the ether gave 6.1 g of 2,3-dihydro-2,2-dimethyl-7-benzofuranyl (methyl)(morpholinosulfenyl)carbamate, m.p. 75° -78° . Recrystallization from hexane-diethyl ether increased the melting point to 89° .

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04006231uspto-grants-1977_02