HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid methylene chloride → N-(3,5-Bis-trifluoromethyl-benzyl)-N-(7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)-acetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | HCID 86616071 | HCID 86616071 | — |
| Product | N-(3,5-Bis-trifluoromethyl-benzyl)-N-(7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)-acetamide | HCID 86616070 | 96% |
Reaction Steps
A solution of (S)-5-[Acetyl-(3,5-bis-trifluoromethyl-benzyl)-amino]-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid tert-butyl ester (0.920 g, 1.50 mmol) (Example 110) in 1:1 TFA/DCM (10.0 ml) was stirred at room temperature for 2 hours. The solvents were evaporated on a (rotary evaporation). Purification by silica gel chromatography (gradient eluent, 0-30% ethyl acetate in hexane) provided the titled compound (0.736 g, 96%) as white solid. MS (ES+): 513 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07749992B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-bbc403dc0ebc4b5b82dd536fe27c1d91 |
| Source note | uspto-grants-2010_07 |