HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid monohydrate → HCID 15583183, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 15583182 | HCID 15583182 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 15583183 | HCID 15583183 | 53% |
Reaction Steps
A mixture of 5.30 g of 3-allyl-2-[2-(3-chloropropionyl)hydrazino]quinazolin-4(3H)-one (0.0173 mol) and 10 mg of p-toluenesulfonic acid hydrate in 300 ml of ethanol was refluxed for 17 hours until TLC indicated that no starting material remained. The mixture was evaporated to dryness and the remaining yellow oil was dissolved in dichloromethane. The solution was washed twice with water, dried over MgSO4, filtered and evaporated. The resulting solid was purified by column chromatography using Kieselgel 60 with CH2Cl2 +1% MeOH as eluant and then was finally crystallized from ethanol to obtain 2.625 g (53% yield) of 4-allyl-1-(2-chloroethyl)[1,2,4]triazolo[4,3-a]quinazolin-5(4H)-one melting at 142.5°-144° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04472400 |
| Source dataset | uspto-grants-1984_09 |
| ORD ID | ord-26cf7cee479f4be1a7c7eae72660b9dd |
| Source note | uspto-grants-1984_09 |