HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → 9-Chloro-7-[2-(2,4-di-t-amylphenoxy)butanoylamino]-6-hydroxy-1,5-benzodiazepin-2,4-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Dimethylacetamide | HCID 31374 | — |
| Reactant | 2-{2-(2,4-Di-t-amylphenoxy)butanamido}-4-chloro-5-aminophenol | HCID 20036192 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 9-Chloro-7-[2-(2,4-di-t-amylphenoxy)butanoylamino]-6-hydroxy-1,5-benzodiazepin-2,4-dione | HCID 135583124 | — |
Reaction Steps
In a mixture of 160 ml of acetonitrile and 20 ml of dimethylacetamide was dispersed 40 g of the 5-amino-4-chloro-2-[2-(2,4-di-t-amylphenoxy)butanoylamino]phenol prepared in (1) above, and 6.6 ml of acetyl chloride was added dropwise thereto while refluxing. After stirring while refluxing for 1 hour, the reaction mixture was cooled. The precipitated crystals were collected by filtration and dried to provide 40.8 g of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04746602 |
| Source dataset | uspto-grants-1988_05 |
| ORD ID | ord-2c971836e8e54c8b9d80a884d4a77f43 |
| Source note | uspto-grants-1988_05 |