HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → HCID 11998031, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-(5-Methyl-1,2-oxazol-3-yl)methanamine | HCID 2776306 | — |
| Reactant | 2,2,2-trichloro-1-{10-[(2,2',6'-trimethyl-1,1'-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone | HCID 68687149 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 11998031 | HCID 11998031 | — |
Reaction Steps
The title compound was prepared according to the procedure of Example 2 starting from 2,2,2-trichloro-1-{10-[(2,2′,6′-trimethyl-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone of Example 3 (1.8 g, 3.26 mmole), (5-methyl-3-isoxazolyl)methylamine (0.305 g, 2.7 mmole), dimethylsulfoxide (1.06 g, 13.6 mmole), and triethylamine (0.605 g, 6 mmole) in 20 mL of acetonitrile. The residue was flash chromatographed on silica Merck-60 using a gradient from 0 to 35% of ethyl acetate in dichloromethane, to provide an orange-yellow foam. Recrystallization from ethyl acetate/dichloromethane/hexane gave a white powder (0.334 g), m.p. 233-234° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07687623B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-42f29be9eb234ca8a63ef032b47f1747 |
| Source note | uspto-grants-2010_03 |