Reaction #302890

ord-6d25758682194a3e9cb055f2726f3e52

Solvents

Conditions

Temperature
80°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Otherwas placed in a sealed reaction vial
  2. 2
    Temperatureto cool
  3. 3
    Othera solid precipitate that had formed
  4. 4
    Filtrationwas collected by filtration
  5. 5
    WashThe solid was rinsed with diethyl ether
  6. 6
    Otherwas dried under reduced pressure

Procedure

A mixture of 0.5 gram (0.0028 mole) of 2,3-dichlorobenzylamine and 0.27 gram (0.0081 mole) of 2-chloroethylisothiocyanate in 10 mL of 1,4-dioxane was placed in a sealed reaction vial. The reaction mixture was heated to 80° C. where it stirred for about 18 hours. The reaction mixture was allowed to cool and a solid precipitate that had formed was collected by filtration. The solid was rinsed with diethyl ether and was dried under reduced pressure to yield 0.68 gram of the title compound. The NMR spectrum was consistent with the proposed structure.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08193118B2uspto-grants-2012_06