HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 131722285, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 21262623 | HCID 21262623 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 131722285 | HCID 131722285 | — |
Reaction Steps
3.53 g (9.0 mmol) of 4-(3-chloroanilino)-6-(4-ethoxycarbonylphenyl)-7H-pyrrolo[2,3-d]pyrimidine are suspended in 150 ml of THF. At 54° C., a total of 0.845 g (21.6 mmol) of lithium aluminum hydride are introduced in the course of 5 h. For working up, 1 ml of water, 2 ml of 1N sodium hydroxide solution and 1 ml of water, followed by 10 g of sodium sulfate, are added successively. The solid is filtered off and the filtrate is concentrated. The residue obtained is washed with methanol and diethyl ether and then dried. 4-(3-Chloroanilino)-6-(4-hydroxymethlyphenyl)-7H-pyrrolo[2,3-d]pyrimidine is obtained in colorless crystals; m.p.>250° C.; FAB-MS (M+H)+=351.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06180636B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-9e35985b60854b3f9b2c9aac3254c3e8 |
| Source note | uspto-grants-2001_01 |