HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → Ammonia methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2-isopropyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine | HCID 21093485 | — |
| Reactant | (S)-2-(2-(3-Fluoro-phenyl)-ethyl)-piperazine | HCID 21093648 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | Ammonia methanol | HCID 21705897 | — |
| Product | (S)-11-{3-[2-(3-Fluoro-phenyl)-ethyl]-piperazin-1-yl}-2-isopropyl-5H-dibenzo[b,e][1,4]diazepine | HCID 58860718 | — |
Reaction Steps
Combine 2-isopropyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine (0.665 g, 2.31 mmol) and (S)-2-[2-(3-fluoro-phenyl)-ethyl]-piperazine (0.962 g, 4.62 mmol)in toluene (4.0 mL) and DMSO (1.0 mL) and heat at 110° C. for 18 hours. Cool to ambient temperature and dilute with ethyl acetate (75 mL). Wash with 0.1N NaOH solution, water and evaporate to give 0.996 g of the crude product. Silica gel chromatography, eluting with methylene chloride: 2N NH3/methanol (100:4), gives 0.216 g of the title compound as a tan solid: mass spectrum (ion spray): n/z=443 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07214673B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-eab96f954eba436ca00721b45940792c |
| Source note | uspto-grants-2007_05 |