HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → 6-aminocarbonyl-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | 4-(3-chloroanilino)-6-ethoxycarbonyl-7H-pyrrolo[2,3-d]pyrimidine | HCID 21262622 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 6-aminocarbonyl-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine | HCID 21262675 | — |
Reaktionsschritte
90 mg (0.285 mmol) of 4-(3-chloroanilino)-6-ethoxycarbonyl-7H-pyrrolo-[2,3-d]pyrimidine (stage 1.4) in 30 ml of methanol and≈5 g of ammonia are heated at 120° C. for 48 h in an autoclave. The reaction mixture is treated with silica gel, evaporated, applied to a silica gel column as a powder and finally eluted with methylene chloride/methanol/THF (210:35:10). Filtration with methanol through an alumina column (basic) and stirring in ethyl acetate yields 6-aminocarbonyl-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine; HPLC: tRet(Grad20)=8.1; TLC-Rf=0.18 (CH2Cl2/methanol [10:1]); high resolution MS: (M+H)+=288.0669 (calc. 288.0652).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06180636B2 |
| Quelldatensatz | uspto-grants-2001_01 |
| ORD ID | ord-322b80f700a349c1b76cea190c98c2be |
| Quellennotiz | uspto-grants-2001_01 |