HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tetrahydrofuran → 5-Amino-7,8-dihydro-2-(methylphenylamino)-7-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | 2-Ethylpropanedioyl dichloride | HCID 10920924 | — |
| Edukt | 4-Amino-2-(methylphenylamino)-5-pyrimidine-carbonitrile | HCID 12784089 | — |
| Produkt | 5-Amino-7,8-dihydro-2-(methylphenylamino)-7-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester | HCID 12784113 | — |
Reaktionsschritte
To 10 g. (0.044 moles) of 4-amino-2-(methylphenylamino)-5-pyrimidine-carbonitrile in 200 ml. of tetrahydrofuran was added 6.7 g. (0.044 moles) of ethyl malonyl chloride and then this mixture was heated at reflux for 2 hours. The reaction was then filtered and the filtercake rinsed with tetrahydrofuran. The filtrate was evaporated to dryness on a rotary evaporator. The viscous liquid residue was treated with 50 ml. of 20% NaOH and heated to boiling for 5 minutes. The resulting solid was removed by filtration. This solid was slurried in water, acidified with acetic acid and filtered. The crude product was recrystallized from 95% ethanol to give 1.05 g. of solid with m.p. 297° C. (dec.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04255568 |
| Quelldatensatz | uspto-grants-1981_03 |
| ORD ID | ord-1535e8895db3439889bbd7d2f7e1d29d |
| Quellennotiz | uspto-grants-1981_03 |