HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 1,1-Dimethylethyl 3,4-dihydro-5-(hydroxymethyl)-2(1H)-isoquinolinecarboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | Sodium borohydride | HCID 4311764 | — |
| Edukt | Tert-butyl 5-formyl-1,2,3,4-tetrahydroisoquinoline-2-carboxylate | HCID 22335239 | — |
| Lösungsmittel | MeOH tetrahydrofuran | HCID 21899815 | — |
| Produkt | 1,1-Dimethylethyl 3,4-dihydro-5-(hydroxymethyl)-2(1H)-isoquinolinecarboxylate | HCID 69561216 | 68,8% |
Reaktionsschritte
To solution of 5-formyl-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester 20a (0.44 g, 1.71 mmol) in 40 mL of methanol:tetrahydrofuran (1:1) at room temperature was added sodium borohydride (0.072 g, 1.88 mmol), and the mixture was stirred to room temperature for 3 h. Water (30 mL) was added followed by ammonium chloride saturated solution (20 mL) and the product was extracted with dichloromethane. The combined organics were dried over magnesium sulfate, the solvent was evaporated and the residue was purified by flash chromatography eluting with 30% ethyl acetate in hexanes, to yield 0.31 g of 5-hydroxymethyl-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester 21a.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07091200B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-b8ea807d82c04522b1c9cb4cd3a35d20 |
| Quellennotiz | uspto-grants-2006_08 |