HuagongsheHuagongshe Chemistry Print Report · For research reference only
Allylamine → 1,1a,2,8,8a,8b-Hexahydro-8-(hydroxymethyl)-8a-methoxy-5-methyl-6-allylamino-azirino[2',3':3,4]pyrrolo-[1,2-a]indole-4,7-dione carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Allylamine | HCID 7853 | — |
| Reactant | Mitomycin A | HCID 19972 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1,1a,2,8,8a,8b-Hexahydro-8-(hydroxymethyl)-8a-methoxy-5-methyl-6-allylamino-azirino[2',3':3,4]pyrrolo-[1,2-a]indole-4,7-dione carbamate | HCID 86737740 | 52.8% |
Reaction Steps
To a solution of 100 mg (0.28 mmol) of mitomycin A in 8 ml of anhydrous methanol, 150 mg (2.6 mmol) of allylamine was added with constant stirring. The reaction mixture was stirred overnight whereupon TLC indicated the absence of starting material. The solvent was then evaporated under reduced pressure and the residue was chromatographed using silica-gel as adsorbent. The fraction obtained by eluting the column from ethyl acetate was evaporated under reduced pressure. Recrystallization from a mixture of methylene chloride and hexane gave 29 mg (27.0% yield) of the desired product as purple-colored crystals having a melting point of 81°-82° (decomposing) and providing the following analysis:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04885304 |
| Source dataset | uspto-grants-1989_12 |
| ORD ID | ord-16a35ad9e8e9478d83cb6cfa76ba86dc |
| Source note | uspto-grants-1989_12 |