Reaction #1247

ord-58e35fa5d3104b07bb1cd637b9c2a80b

Reaction equation

O=C1CCCO1
γ-butyrolactone
[Cl-].[NH4+]
ammonium chloride
CC(CN)(CN)CN
1,1,1-tris(aminomethyl)ethane
CC1(CN)CN=C2CCCN2C1
amine
CC1(CN)CN=C2CCCN2C1
3-(aminomethyl)-3-methyl-2,3,4,6,7,8-hexahydropyrrolo[1,2-a]pyrimidine

Solvents

Conditions

Temperature
250°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturethe mixture was cooled

Procedure

A mixture of 21.03 g (0.24 mol) of γ-butyrolactone and 1.31 g (24 mmol) of ammonium chloride in 114.5 g (0.98 mol) of 1,1,1-tris(aminomethyl)ethane was heated at 250° C. in an autoclave. After 1.5 h, the mixture was cooled and the excess amine and the water formed were removed by distillation. The residue was distilled at 200°-240° C./18 mbar. The yield was 22.0 g (54%) of yellowish oil. The boiling point was 117°-120° C./1 mbar. Other data concerning the product was:

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05723605uspto-grants-1998_03