Reaktion #171920
ord-1d3a3d8d9a7a475cb0d380c88f42c3f3
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas heated
- 2Temperaturto reflux for 48 h
- 3Sonstigequenched by MeOH
- 4SonstigeThe volatile was removed under vacuum
- 5workup.ADDITION2 N HCl (100 mL) was added to the residue
- 6Temperaturheated
- 7Temperaturto reflux for 18 h
- 8SonstigeSolvent 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.