HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 18931068, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2-Thiophenesulfonyl chloride | HCID 85518 | — |
| Reactant | HCID 18931075 | HCID 18931075 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18931068 | HCID 18931068 | 58.2% |
Reaction Steps
A mixture of 4-amino-6-[2-(5-bromopyrimidin-2-yloxy)ethoxy]-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-pyrimidine (100 mg), sodium hydride (60 dispersion, 53.5 mg) and tetrahydrofuran (3 ml) is stirred at room temperature for 20 minutes. To the mixture is added thiophenesulfonyl chloride (23.4 mg), and the mixture is stirred for 22 hours. The reaction solution is treated with a saturated aqueous ammonium chloride solution, and extracted with ethyl acetate. The ethyl acetate layer is washed, dried, and evaporated under reduced pressure to remove the solvent. The residue is purified by preparative thin layer chromatography (solvent; chloroform: methanol=10:1) to give the title compound (49.1 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05739333 |
| Source dataset | uspto-grants-1998_04 |
| ORD ID | ord-6b476f5c5d9d4dab8dd1084355d5682f |
| Source note | uspto-grants-1998_04 |