HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 22105475, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 22105470 | HCID 22105470 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22105475 | HCID 22105475 | — |
Reaction Steps
A solution of methyl amine (16.0 mL of a 1.1N THF solution, 17.6 mmole) in 50 mL of dry THF was cooled to 0°-5° C. in an ice-water bath. To this solution was added, over a ten minute period, a solution of crude rac-3-bromo-7-chloro-5-(2-chlorophenyl)-1,3-dihydro-2-H1-benzazepin-2-one (3.36 g estimated to be 85% pure, 7.36 mmole), dissolved in 55 mL of THF. After 10 minutes, the reaction solution was diluted with 300 mL of EtOAc, washed with water and brine, and dried (sodium sulfate). Concentration and drying under high vacuum yielded 2.98 g of crude material, which was used as is in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05843941 |
| Source dataset | uspto-grants-1998_12 |
| ORD ID | ord-887de6470d144231b3f768ee422702b2 |
| Source note | uspto-grants-1998_12 |