HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → 1,3-dimethyl-6-[4-(3-[2-hydroxy-5-nitrophenyloxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | 1,3-dimethyl-6-[4-(3-hydroxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione | HCID 10356417 | — |
| Reactant | HCID 19011773 | HCID 19011773 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1,3-dimethyl-6-[4-(3-[2-hydroxy-5-nitrophenyloxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione | HCID 19011908 | 43.8% |
Reaction Steps
In 15 ml of anhydrous tetrahydrofuran were suspended 0.63 g of 2-nitrocatechol, 1.0 g of 1,3-dimethyl-6-[4-(3-hydroxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione (Compound a) and 1.06 g of triphenylphosphine, and 0.71 g of diethyl azodicarboxylate was added to the resultant suspension. Afterward, the resultant mixture was treated in the same manner as in Reference Example 4 to obtain 0.65 g of light yellow crystals. The crystals were recrystallized from ethanol to obtain 0.55 g of crystalline 1,3-dimethyl-6-[4-(3-[2-hydroxy-5-nitrophenyloxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione (Compound y).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05332739 |
| Source dataset | uspto-grants-1994_07 |
| ORD ID | ord-5e6fa889999c49bba1b8ab57b6e47d94 |
| Source note | uspto-grants-1994_07 |