HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 10-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H,11aH)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | 2,3-Dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H,11ah)-dione | HCID 551139 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 10-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H,11aH)-dione | HCID 9859436 | — |
Reaction Steps
A mixture of 4.32 g. of 1,2,3,11a-tetrahydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-5,11(10H)-dione, 1.2 g. of sodium methylate and 40 ml. of ethanol is stirred at room temperature for 3 hours and 3 ml. of methyl iodide is added. The reaction mixture is stirred for 16 hours longer and concentrated. The residue is mixed with benzene and water and the layers are separated. The benzene layer is washed with water and concentrated. The product is further purified by recrystallization from ethyl acetate and melts at 124°-126° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03985732 |
| Source dataset | uspto-grants-1976_10 |
| ORD ID | ord-1d61152a66ed46259265c4ee62255df7 |
| Source note | uspto-grants-1976_10 |