HuagongsheHuagongshe Chemistry Print Report · For research reference only
Mechlorethamine → 1-Methyl-4-phenylpiperidine-4-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Mechlorethamine | HCID 4033 | — |
| Reactant | Phenylacetonitrile | HCID 8794 | — |
| Reactant | Sodium amide | HCID 24533 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 1-Methyl-4-phenylpiperidine-4-carbonitrile | HCID 62513 | 58.5% |
Reaction Steps
To a solution of mechlorethamine (4 g, 25.6 mmol) and benzyl cyanide (4 g, 34.2 mmol) in toluene (25 ml) was added sodium amide (2 g, 51.2 mmol) at 40-50° C. in portions for 1 hour. The reaction mixture was heated to reflux about 2 hours after the addition. The reaction mixture was cooled to room temperature and washed with saturated sodium bicarbonate solution and brine, dried over sodium sulfate and concentrated. The residue was applied to flash column chromatography using methylene chloride and methanol (100:5) as eluents to give 3 g of desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07649092B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-a6b5865b77124f84a75bcab02018e967 |
| Source note | uspto-grants-2010_01 |