HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylbenzoyl Chloride → 1-Benzyl-3-p-tolyl-1,4,5,6,7,8-hexahydro-1,2,6-triaza-azulene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylbenzoyl Chloride | HCID 13405 | — |
| Reactant | JNJ-18038683 free base | HCID 11151899 | — |
| Product | 1-Benzyl-3-p-tolyl-1,4,5,6,7,8-hexahydro-1,2,6-triaza-azulene | HCID 59752563 | 6.3% |
Reaction Steps
The title compound (0.2 g) was prepared from 4-oxo-azepane-1-carboxylic acid tert-butyl ester (Example 59, Step B; 10 mmol) as in Example 59, Steps C through E, using 4-methyl-benzoyl chloride (11 mmol) in place of 4-chloro-benzoyl chloride. MS (ESI): exact mass calculated for C21H23N3, 317.19; found, m/z 318.2 [M+H]+. 1H NMR (500 MHz, CD3OD): 7.34-7.33 (m, 2H), 7.29-7.26 (m, 2H), 7.24-7.21 (m, 3H), 7.10-7.09 (m, 2H), 5.40 (s, 2H), 3.33-3.27 (m, 4H), 3.11-3.09 (m, 2H), 3.00-2.98 (m, 2H), 2.30 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07579470B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-8d92942d49944bc0a2d0b7db7c44eb4a |
| Source note | uspto-grants-2009_08 |