(S)-3-methoxymethylamino-1-(2-thienyl)propan-1-ol → 3-(N-Methylamino)-1-(2-thienyl)-1-propanol, (-)-

(S)-3-methoxymethylamino-1-(2-thienyl)propan-1-ol obtained in example 2 was dissolved in 10 ml of methanol with 8 mg of Raney-nickel. The resulting solution was provided in a glass autoclave and hydrogenated at 50° C. for 12 hours. Upon completion of hydrogenation, the reaction mixture was filtered and the solvent was removed under reduced pressure to obtain the objective compound as a crystal compound (122 mg, 95% ee; purity; 90.8% by HPLC assay). The crude product was further purified by re-crystallization in toluene to give a product with optical purity as high as 100% ee.

1. customThe resulting solution was provided in a glass autoclave and hydrogenated at 50° C. for 12 hours
2. filtrationUpon completion of hydrogenation, the reaction mixture was filtered
3. customthe solvent was removed under reduced pressure

ORD-Eintrag

ord-c3721bdd8b24453ba0fb7ebb7d1121a4

Quelldatensatz

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08957227B2