HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylethylamine → HCID 86762230, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylethylamine | HCID 11723 | — |
| Edukt | Acetonitrile methanol | HCID 21959252 | — |
| Edukt | HCID 89832302 | HCID 89832302 | — |
| Lösungsmittel | Carbon Dioxide | HCID 280 | — |
| Produkt | HCID 86762230 | HCID 86762230 | 37,4% |
Reaktionsschritte
Racemic benzyl 2-benzamido-7a-phenyl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazine-6-carboxylate (30 g, 63 mmol) is chirally purified by SFC: (Column: Chiralpak IC 2.1×25 cm; eluent: 40% methanol/acetonitrile (8/2) with 0.2% dimethylethyl amine in CO2; flow: 70 mL/min at UV 284 nm). The second eluting isomer is the title compound (11.1 g, 37%, >98% ee). Chiral analysis of the isolated isomer 2: Chiralpak IC 0.46×10 cm, 5 μm; eluent: 40% methanol/acetonitrile (8/2) with 0.2% dimethyl ethyl amine in CO2; flow: 5 mL/min at UV 215 nm. Rt=3.2 minutes. [α]D20=−88 (C=1.0, methanol), ES/MS (m/e) 372 (M+H)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08889856B2 |
| Quelldatensatz | uspto-grants-2014_11 |
| ORD ID | ord-b3e03c3bf2a14cd99f884f15258ef18c |
| Quellennotiz | uspto-grants-2014_11 |