HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 7-Methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-6-ol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Hydroxyacetone | HCID 8299 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 4-Amino-2-(methylsulfanyl)pyrimidine-5-carbaldehyde | HCID 295769 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Water ethanol | HCID 19096565 | — |
| Produkt | 7-Methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-6-ol | HCID 89809360 | 56% |
Reaktionsschritte
Add 1-hydroxypropan-2-one (24.3 mL, 355 mmol) and 4-amino-2-(methylthio)pyrimidine-5-carbaldehyde (50 g, 296 mmol) to a solution of sodium hydroxide (23.64 g, 591 mmol) and water (200 mL). Add EtOH (600 mL) to the suspension and stir at RT overnight. Slowly add a solution of concentrated HCl (50 mL) in water (350 mL). Add 1:1 EtOH/H2O (100 mL) and collect the solids by filtration. Wash the solids with 1:1 EtOH/H2O (250 mL), ice cold EtOH (4×25 mL) and hexanes (2×250 mL). Dry in the vacuum oven at 30-35° C. to provide the title compound as a tan solid (34 g, 56% yield). MS (m/z): 208.1 (M+1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09334267B2 |
| Quelldatensatz | uspto-grants-2016_05 |
| ORD ID | ord-3eb8ef251cf0428a967a2a9b4665fc7f |
| Quellennotiz | uspto-grants-2016_05 |