HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 10178894, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Cyclohexylbenzoyl chloride | HCID 21890847 | — |
| Reactant | 10,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepine | HCID 22135237 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10178894 | HCID 10178894 | 83.3% |
Reaction Steps
A solution of 10,11-dihydro-5-methyl-dibenzo[b,e][1,4]diazepine of Step C (0.42 g) in dichloromethane (10 mL) containing N,N-diisopropylethyl amine (0.29 g) was treated with 4-cyclohexylbenzoyl chloride (0.50 g). After stirring overnight at room temperature, the reaction mixture was washed with water and saturated aqueous sodium bicarbonate, then dried over anhydrous sodium sulfate. The solution was filtered through a short column of Magnesol® which was eluted with several additional volumes of dichloromethane. Evaporation of all volatiles gave a glassy residue which was triturated with anhydrous diethyl ether to provide the title compound as an off-white crystalline solid (0.66 g), m.p. 111–112° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07053083B2 |
| Source dataset | uspto-grants-2006_05 |
| ORD ID | ord-d8adca14560d4ca0af74cf25c8665c83 |
| Source note | uspto-grants-2006_05 |