HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 5327740, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | HCID 10096174 | HCID 10096174 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 5327740 | HCID 5327740 | — |
Reaction Steps
200 mg of trifluoromethanesulfonic anhydride in 50 ml of dichloromethane were treated at 0° C. under a nitrogen atmosphere with a suspension of 150 mg of the pyrroledione product of Example 9 and 75 mg of collidine in 50 ml of dichloromethane. After 2 hours, 4 ml of 33% aqueous ammonia were added and the mixture was left to warm to room temperature overnight. The mixture was washed with water, dried and evaporated to dryness. The residue was purified by chromatography on silica gel with dichloromethane/methanol/acetone/water (90:18:3:2). Crystallization from dichloromethane/n-hexane gave 85 mg of 3-[7-(aminomethyl)-6,7,8,9-tetrahydropyrido[1,2-a]indol-10-yl]-4-(1-methyl-3-indolyl)-1H-pyrrole-2,5-dione of melting point 160°-165° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05721245 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-2fd3228342014e298f177ca3c473632b |
| Source note | uspto-grants-1998_02 |