Reaktion #4340

ord-e8648a916c7c4fcfb8175365162e18a3

Reaktionsgleichung

COC(=O)Cl
chloroformic acid methyl ester
CSCCOc1ccccc1NN
2-(2-methylthioethoxy)-phenylhydrazine
O
H2O
COC(=O)NNc1ccccc1OCCSC
2-[2-(methylthioethoxy)-phenyl]-hydrazinecarboxylic acid methyl ester

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe mixture is repeatedly extracted with ethyl acetate
  2. 2
    SonstigeAfter customary further processing, a solid is obtained
  3. 3
    Sonstigethis is recrystallised from alcohol
  4. 4
    Sonstigeto thus yield the compond of the formula

Vorschrift

5.6 ml of chloroformic acid methyl ester are added dropwise at 0° C. to 14.4 g of 2-(2-methylthioethoxy)-phenylhydrazine in 100 ml of tetrahydrofuran and 14 g of N-ethyldiisopropylamine. The reaction mixture is stirred at 20° C. for 2 hours; H2O is then added, and the mixture is repeatedly extracted with ethyl acetate. After customary further processing, a solid is obtained, and this is recrystallised from alcohol to thus yield the compond of the formula ##STR62## having a melting point of 92°-94° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04725302uspto-grants-1988_02