HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 58495446, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 86624171 | HCID 86624171 | — |
| Solvent | Ammonium Hydroxide | HCID 14923 | — |
| Product | HCID 58495446 | HCID 58495446 | 93.2% |
Reaction Steps
Dissolve 7-chloro-6-{4-[(N-methyl-iso-propylamino)-methyl]-benzylamino}-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (350 mg, 0.75 mmol) in concentrated NH4OH. (10 mL) and MeOH (10 mL). Stir the reaction mixture overnight. Concentrate the mixture in vacuo. Purify by chromatography on silica gel (45 g) eluting with a gradient of 100% DCM to 1:1 DCM/(chloroform:methanol:concentrated NH4OH 80:18:2) to obtain 7-chloro-6-{4-[(N-methyl-iso-propylamino)-methyl]-benzylamino}-2,3,4,5-tetrahydro-1H-benzo[d]azepine (260 mg, 93%). MS (APCI+) m/z: 372 (M+11)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680091B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-c4f8c5d21c4e45d78d3ec9eaca2eb330 |
| Source note | uspto-grants-2014_03 |