HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2,3-Dichloro-5-methylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2,4-Dichloro-4-methyl-5-oxopentanenitrile | HCID 13373594 | — |
| Catalyst | Tantalum | HCID 23956 | — |
| Catalyst | Copper | HCID 23978 | — |
| Product | 2,3-Dichloro-5-methylpyridine | HCID 12747761 | 64.8% |
Reaction Steps
18 g of the 4-formyl-2,4-dichlorovaleronitrile obtained in Example 3(a) and 0.1 g of copper powder are heated in a tantalum autoclave for 5 hours to 150° C. after the introduction of 10 g of dry HCl gas under pressure. After they have cooled, the contents of the autoclave are subjected to steam distillation, affording 10.5 g of 2,3-dichloro-5-methylpyridine in the form of colourless crystals with a melting point of 46°-47° C. 1H-NMR spectrum (100 MHz in CDCl3) in ppm: 8.13 (d, 1H, H on C-6); 7.59 (d, 1H, H on C-4); 2.34 (s, 3H, --CH3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04469896 |
| Source dataset | uspto-grants-1984_09 |
| ORD ID | ord-c7ce290b1ec2476ca0c142b0956e5b6b |
| Source note | uspto-grants-1984_09 |