HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-[[3-(4-Methoxyphenyl)-1,2,4-triazolo[3,4-a]phthalazin-6-yl]oxy]-2-pyrrolidinone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3-Bromopyrrolidin-2-one | HCID 10103471 | — |
| Reactant | HCID 178489106 | HCID 178489106 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 3-[[3-(4-Methoxyphenyl)-1,2,4-triazolo[3,4-a]phthalazin-6-yl]oxy]-2-pyrrolidinone | HCID 21283337 | 82% |
Reaction Steps
6-Hydroxy-3-(4-methoxyphenyl)-1,2,4-triazolo[3,4-a]phthalazine, (9.8 g), is suspended in N,N-dimethylformamide (100 ml) and added of 50% sodium hydride in mineral oil (1.7 g). The mixture is heated to 50°-60° C. and stirred for about 2 hours. After cooling to room temperature the mixture is added portionwise with 3-bromo-2-pyrrolidone (5.5 g). [This product is prepared according to F. Korte, H. Wanholf, Ber. 97, 1976 (1964)]. Then stirring is continued for about 5 hours at a temperature of about 70° C. The mixture is then cooled to room temperature and poured into water (800 ml). The residue, which is collected by filtration, is then crystallized from ethanol/chloroform. (Yield=82%). M.p. 290°-293° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04788186 |
| Source dataset | uspto-grants-1988_11 |
| ORD ID | ord-ef3962880fda4ae38f769bfeea5a2600 |
| Source note | uspto-grants-1988_11 |