HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosgene → HCID 22125063, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosgene | HCID 6371 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 22125127 | HCID 22125127 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22125063 | HCID 22125063 | 83% |
Reaction Steps
A mixture of 240 mg (1 mmol) of 5-tert.butylaminomethyl-4-methylamino-2-methylthiopyrimidine and 0.28 ml of triethylamine in 5 ml of tetrahydrofuran was added dropwise to an ice-cooled solution of 1 ml (1.92 mmol) of phosgene (20% solution in toluene) in 5 ml of tetrahydrofuran. After 1 hour 30 ml of saturated aqueous ammonium chloride and 20 ml of tetrahydrofuran were added to the resulting mixture. The phases were separated. The organic phase was dried over magnesium sulfate, filtered and then evaporated to give 220 mg (83%) of 3-tert.butyl-7-methylthio-3,4-dihydro-1-methylpyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06150373 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-f19d01b856634e6284350401e22e247d |
| Source note | uspto-grants-2000_11 |