HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 10229346, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1-Methylhomopiperazine | HCID 228349 | — |
| Reactant | HCID 10223535 | HCID 10223535 | — |
| Reactant | HCID 18449085 | HCID 18449085 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10229346 | HCID 10229346 | — |
Reaction Steps
The crude 10-(4-cyclohexyl-benzoyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carbonyl chloride (prepared from 2.5 g of the corresponding acid of Example 22, in the manner of Example 23) was added to a stirred mixture of N,N-diisopropylethyl amine (1.73 g), 4-(dimethylamino)pyridine (0.1 g) and N-methyl homopiperazine (1.52 g) in dichloromethane (25 mL). After stirring overnight at room temperature the reaction mixture was washed with water and saturated aqueous sodium bicarbonate, and dried over anhydrous sodium sulfate. The solution was filtered through a short column of Magnesol® and the eluate refluxed with the slow addition of hexane to provide the title compound as off-white crystals (0.46 g), m.p. 133–136° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07202239B2 |
| Source dataset | uspto-grants-2007_04 |
| ORD ID | ord-85b5d41bf34945509c5232b06b0d5e09 |
| Source note | uspto-grants-2007_04 |