HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23282691, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 23282721 | HCID 23282721 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 23282691 | HCID 23282691 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
For the preparation of the HCl salt, 600 mg of 4-(3-chloro-anilino)-5-methyl-6-(4-hydroxy-phenyl)-7H-pyrrolo[2,3-d]pyrimidine hydrobromide are dissolved while hot in 50 ml of ethyl acetate and at RT adjusted to pH 9.5 with 1 N NaOH and the organic phase is washed twice with water. The organic phase is dried and concentrated by evaporation, and the residue is dissolved in 30 ml of ethanol, and a 5N (=5 normal) ethanolic HCl solution is added thereto. At 0° C., with stirring and the addition of diethyl ether, 4-(3-chloro-anilino)-5-methyl-6-(4-hydroxyphenyl)-7H-pyrrolo[2,3-d]pyrimidine hydrochloride is obtained in the form of a colourless powder having a m.p. of 280-282° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06140332 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-e0f279993fce413cb16165e4d9d03e19 |
| Source note | uspto-grants-2000_10 |