HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 21254924, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 21255049 | HCID 21255049 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21254924 | HCID 21254924 | 63% |
Reaction Steps
10 ml of a 50% solution of NH3 in MeOH were added to a solution of 0.50 g (1.25 mmol) of 3-benzenesulphonyl-7-chloro-5-(2-methoxy-ethyl)-2-methylsulphanyl-pyrazolo[1,5-a]-pyrimidine in 10 ml of DMF and stirred at RT for 2 hrs. The reaction solution was evaporated in a high vacuum and the residue was partitioned between 2N NaOH and CH2Cl2. The aqueous phase was extracted three times with CH2Cl2 and the combined organic phases were dried (MgSO4), filtered and evaporated. Subsequent chromatography (SiO2, CH2Cl2/MeOH 10:1) and crystallization from EtOH yielded 0.30 g (63%) of 3-benzenesulphonyl-5-(2-methoxy-ethyl)-2-methylsulphanyl-pyrazolo[1,5-a]pyrimidin-7-ylamine as colorless crystals, m.p. 186-187°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06194410B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-698157bc1a1d4674bb020be51d4fb2ce |
| Source note | uspto-grants-2001_02 |