Reaktion #1135797

ord-dcc38955e6714627b69d85307b2d3c3a

Reaktionsgleichung

COC(=O)Cl
methyl chloroformate
C1CCOC1
tetrahydrofuran
Cc1c(N)cccc1Cl
1-chloro-2-methyl-3-aminobenzene
COC(=O)Nc1cccc(Cl)c1C
1-chloro-2-methyl-3-methoxycarbonylaminobenzene

Lösungsmittel

Reaktionsbedingungen

Temperatur
25°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo the reaction mixtures
  2. 2
    Extraktionthe resulting mixtures were extracted with ethyl acetate
  3. 3
    WaschenThe organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    Trocknenwere dried over anhydrous sodium sulfate
  5. 5
    EinengenThe mixtures were concentrated under reduced pressure

Vorschrift

Under cooling, to a mixture of methyl chloroformate 30 mL and tetrahydrofuran 50 mL was added dropwise 1-chloro-2-methyl-3-aminobenzene 5.00 g and the mixtures were stirred at 25° C. for a half hour. To the reaction mixtures was added water and the resulting mixtures were extracted with ethyl acetate. The organic layers were washed with aqueous saturated sodium bicarbonate solution and were dried over anhydrous sodium sulfate. The mixtures were concentrated under reduced pressure to give 1-chloro-2-methyl-3-methoxycarbonylaminobenzene 5.80 g.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09380782B2uspto-grants-2016_07