HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenyl isocyanate → US10752598, Example 20
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenyl isocyanate | HCID 7672 | — |
| Reactant | 3-Amino-1-phenyl-1,5-dihydrobenzo[b][1,4] diazepine-2,4-dione | HCID 10683252 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | US10752598, Example 20 | HCID 10667855 | 71.9% |
Reaction Steps
To a slurry of 3-amino-1-phenyl-1,5-dihydro-benzo [b] [1,4]-diazepine-2,4-dione (0.398 g) in dichloromethane (5 ml) was added phenyl isocyanate (0.177 g) gradually with stirring at ambient temperature. The reaction mixture was stirred two hours at ambient temperature after which time a cream precipitate was separated by filtration to provide the title compound (0.413 g). 1H NMR (300 MHz, DMSO-d6): d 4.97 (d, J=7.5 Hz, 1H), 6.88-6.97 (m, 3H), 7.13-7.47 (m, 12H), 9.16 (s, 1H), 10.78 (br s, 1H); TLC (CH2Cl2 /CH3OH,19:1): Rf =0.21
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05910495 |
| Source dataset | uspto-grants-1999_06 |
| ORD ID | ord-e7094706bf4d4cb3bf2094393b2e0610 |
| Source note | uspto-grants-1999_06 |