HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-(3-(N-(5-chloropentanoyl)amino)phenyl)-5,6,7,8-tetrahydrophthalazin-1(2H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-Chlorovaleryl chloride | HCID 74089 | — |
| Reactant | 4-(3-aminophenyl)-5,6,7,8-tetrahydrophthalazin-1(2H)-one | HCID 23032581 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(3-(N-(5-chloropentanoyl)amino)phenyl)-5,6,7,8-tetrahydrophthalazin-1(2H)-one | HCID 66966351 | — |
Reaction Steps
5-chloropentanoyl chloride (171 mg) was added dropwise to a mixed solution of the compound prepared in Example 1 (241 mg) and potassium carbonate (89.8 mg) in tetrahydrofuran (3.00 mL) and water (1.00 mL) in ice bath and the mixture was stirred for 30 minutes. Moreover, potassium carbonate (45.0 mg) and 5-chloropentanoyl chloride (85.5 mg) was added the reaction mixture, which was stirred for 30 minutes. 1N hydrochloric acid was added to the reaction mixture, which was adjusted to pH 2. Water was added thereto and the deposited crystal was collected by filtration. It was washed with water and hexane sequentially and dried under reduced pressure to give the compound of the present invention (347 mg) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07402580B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-6f715311f9a44c5f9a1ca337bf778988 |
| Source note | uspto-grants-2008_07 |