HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine hydrochloride → HCID 59287395, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine hydrochloride | HCID 11130 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 59287378 | HCID 59287378 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 59287395 | HCID 59287395 | 67.3% |
Reaction Conditions
| Temperature | 160 °C |
|---|
Reaction Steps
2-Amino-6-methoxymethyl-nicotinonitrile (0.20 g) described in Manufacturing Example 6-2, sodium azide (0.40 g), triethylamine hydrochloride (1.7 g), and NMP (25 mL) were stirred for 2 hours at 160° C. The reaction solution was directly purified by silica gel chromatography (ethyl acetate, then ethyl acetate:methanol:concentrated aqueous ammonia=6:2:1). The organic layer thus obtained was concentrated and purified by silica gel chromatography (ethyl acetate:methanol=4:1) to obtain the titled compound (170 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183264B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-0477054c7a9f481785574833ca88f8e6 |
| Source note | uspto-grants-2012_05 |