HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 74389-71-2
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | 1H-1,5-Benzodiazepin-2-one, 2,3,4,5-tetrahydro-4-methyl- | HCID 19868 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 74389-71-2 | HCID 3033608 | 83.2% |
Reaction Steps
A solution of 4-methyl-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (220 mg, 1.25 mmol) and P2S5 (444 mg, 2.0 mmol) in pyridine (10 mL) was heated at 120° C. for 30 min. To the mixture, water (10 mL) was added, and then extracted with ethyl acetate (20 mL), dried with Na2SO4, concentrated and purified by CombiFlash (PE:EA=10:1) to give 4-methyl-4,5-dihydro-1H-benzo[b][1,4]diazepine-2(3H)-thione (200 mg, 83%). LRMS (M+H)+: 192 m/z.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09422292B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-4d28bc507c8547a1a2a97fd444b2c2ca |
| Source note | uspto-grants-2016_08 |