HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 86711623, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | HCID 86711622 | HCID 86711622 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86711623 | HCID 86711623 | — |
Reaction Steps
Hydrazine (85% in water, 2.0 g, 53 mmol) is added to a solution of 2-(3-fluoro-4-(N-cyano-S-methylsulfonimidoyl)-benzyl)-isoindole-1,3-dione (preparation 15c, 3.5 g, 8.8 mmol) in a 1:1 mixture of dichloromethane and methanol (140 mL). The mixture is stirred over night and concentrated under reduced pressure. The residue is purified by preparative reversed phase HPLC (Luna C18(2), gradient of acetonitrile in water, 0.01 M NH3). Yield: 1.2 g (58% of theory); ESI mass spectrum: [M+H]+=228; r.t. HPLC: 0.26 min (X011_S03).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09346794B1 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-d4d841b3d4dd4508a0d9c37101a450dc |
| Source note | uspto-grants-2016_05 |