Reaction #2171026

ord-36cbbf916d1542eab4aa0b916cc6c6eb

Solvents

Conditions

Temperature
50°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.ADDITIONare added drop-wise within 20 minutes
  2. 2
    OtherAfter about 10 minutes further crystallization
  3. 3
    Filtrationa precipitate that appears is filtered with suction
  4. 4
    WashAfter washing with a little cold methanol the precipitate
  5. 5
    Otheris dried under vacuum

Procedure

To a suspension of 102 g terephthaldehyde in 700 ml methanol 129.4 g of 2-cyanoethylhydrazine are added drop-wise within 20 minutes. The temperature increases to about 50° C., and an orange-red solution generally arises. After about 10 minutes further crystallization occurs. Stirring continues for 30 minutes and a precipitate that appears is filtered with suction. After washing with a little cold methanol the precipitate is dried under vacuum. 187 g of beige colored product are produced.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06716257B2uspto-grants-2004_04