HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 178526611, compound → HCID 178507540, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 178526611 | HCID 178526611 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178507540 | HCID 178507540 | — |
Reaction Steps
In the presence of 30 mg of Raney nickel, 110 mg (0.30 mmol) of 3-(3-nitro-phenyl)-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine are hydrogenated in 3 ml of methanol and 3 ml of THF. The catalyst is filtered off, then 15 g of silica gel are added to the filtrate, which is then concentrated by evaporation. Application of the powder to a silica gel column, elution with methylene chloride/ethanol (15:1) and stirring of the crude product with diethyl ether/hexane yield 3-(3-amino-phenyl)-4-(3-chloro-phenylamino)-1H-pyrazolo-[3,4-d]pyrimidine; m.p. 264-266° C.; TLC: Rf =0.45 (methylene chloride/methanol 10:1); HPLC: TRet (Grad20-100)=9.7.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05981533 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-de65481f771b42c7b7c3073b2db127f7 |
| Source note | uspto-grants-1999_11 |