HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 86752155, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | HCID 10004096 | HCID 10004096 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86752155 | HCID 86752155 | — |
Reaction Steps
546 mg of trifluoromethanesulphonic anhydride in 80 ml of dichloromethane were treated at 0° C. under a nitrogen atmosphere with a suspension of 400 mg of the product of Example 19 and 208 mg of collidine in 120 ml of dichloromethane. After 1 hour, 1.9 ml of 40% aqueous dimethylamine were added and the mixture was stirred for 3 hours. The solvent was removed and the residue was subjected to chromatography on silica gel with dichloromethane/methanol/acetone (88:10:2). Trituration with ethyl acetate followed by recrystallization from methanol gave 295 mg of 3-[2,3-dihydro-2-(dimethylaminomethyl)-1H-pyrrolo[1,2-a]indol-9-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione trifluoromethanesulphonate of melting point 323°-325° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05721245 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-beabd9295e7e47d1b875145e56da89a1 |
| Source note | uspto-grants-1998_02 |