HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 54101464, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Cyanide | HCID 8929 | — |
| Reactant | HCID 20637716 | HCID 20637716 | — |
| Solvent | Methylamine | HCID 6329 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54101464 | HCID 54101464 | — |
Reaction Steps
In a bomb tube, 155 mg (0.50 mmol) of 6-ethoxycarbonyl-4-[1(R)-phenyl-ethylamino]-7H-pyrrolo[2,3-d]pyrimidine and 2.5 mg (0.05 mmol) of NaCN in 4 ml of methylamine (33% in ethanol) are heated at 50° C. for 30 hours. The reaction mixture is dissolved in THF, 25 ml of water are added thereto and concentration by evaporation is carried out to a residual volume of =25 ml. The resulting crystals are filtered off and washed with water. Recrystallization from hot THF and ethyl acetate yields the title compound; HPLC: tRet (Grad20)=8.3; TLC-Rf =0.31 (CH2Cl2 /methanol [10:1]); FAB-MS: (M+H)+ =296.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06140332 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-fd8befb2293847678577d9644014c703 |
| Source note | uspto-grants-2000_10 |