HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 67263977, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 86633916 | HCID 86633916 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67263977 | HCID 67263977 | 77.8% |
Reaction Steps
A mixture of 7-Methoxy-1-methyl-8-nitro-4-(2,2,2-trifluoro-acetyl)-1,3,4,5-tetrahydro-benzo[e][1,4]diazepin-2-one (2.86 g, 0.00824 mol) and 7.0 M of Ammonia in Methanol (30 mL) were reacted in an analogous manner to example 736-D to give an oil. 7-Methoxy-1-methyl-8-nitro-1,3,4,5-tetrahydro[e][1,4]diazepin-2-one It was triturated with diethyl ether giving 7-Methoxy-1-methyl-8-nitro-1,3,4,5-tetrahydro-benzo[e][1,4]diazepin-2-one as a tan solid (1.61 g, 77%). Mp 145-149° C.; LCMS (m/e) 252 (M+1); 1H-NMR (DMSO, 400 MHz) δ 7.91 (s, 1H), 7.41 (s, 1H), 3.94 (s, 2H), 3.79 (s, 1H), 3.31 (s, 3H), 3.25 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08148391B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-9116e04c57534f5492105a1f76f78bda |
| Source note | uspto-grants-2012_04 |