HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide dimethyl acetal → HCID 22605454, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Reactant | HCID 9949425 | HCID 9949425 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22605454 | HCID 22605454 | — |
Reaction Steps
A mixture of 4-(5H,11H-pyrrolo[2,1-c][1,4]benzodiazepine-10-carbonyl)-benzamide (1.25 g) from Example 45 and dimethylformamide dimethylacetal (20 ml) was refluxed for 4 hours and the volatiles removed in vacuo to give a solid. The solid was dissolved in dichloromethane and filtered through a short column of hydrous sodium magnesium silicate and further eluted with several volumes of dichloromethane. The combined organic phase was concentrated on a steam bath with the gradual addition of hexane until crystallization occurred. After cooling, the crystals were collected by filtration to yield the title compound (1.40 g), m.p. 232-234° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06831079B1 |
| Source dataset | uspto-grants-2004_12 |
| ORD ID | ord-8aa7b50248934748856974e46606e7c2 |
| Source note | uspto-grants-2004_12 |