Reaktion #171920

ord-1d3a3d8d9a7a475cb0d380c88f42c3f3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturto reflux for 48 h
  3. 3
    Sonstigequenched by MeOH
  4. 4
    SonstigeThe volatile was removed under vacuum
  5. 5
    workup.ADDITION2 N HCl (100 mL) was added to the residue
  6. 6
    Temperaturheated
  7. 7
    Temperaturto reflux for 18 h
  8. 8
    SonstigeSolvent was removed under vacuum

Vorschrift

A mixture of 2-Amino-1-(1,1-dioxo-llambda*6*-thiomorpholin-4-yl)-propan-1-one (6.0 g, 18.2 mmol) and BH3 (1 M in THF, 110 mL) was heated to reflux for 48 h, then cooled to room temperature and quenched by MeOH. The volatile was removed under vacuum. 2 N HCl (100 mL) was added to the residue and heated to reflux for 18 h. Solvent was removed under vacuum to give (S)-2-(1,1-Dioxo-llambda*6*-thiomorpholin-4-yl)-1-methyl-ethylamine (4.5 g) as white solid, yield 90%. MS (M+H)=193.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846945B2uspto-grants-2014_09