HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 5-Tert-butyl-2-methoxy-3-nitrobenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Trimethylsilyldiazomethane | HCID 167693 | — |
| Reactant | 5-Tert-butyl-2-hydroxyl-3-nitro-benzonitrile | HCID 58980653 | — |
| Solvent | Acetonitrile methanol | HCID 21959252 | — |
| Product | 5-Tert-butyl-2-methoxy-3-nitrobenzonitrile | HCID 50883199 | 99.9% |
Reaction Steps
The above nitrile (0.5 g, 2.27 mmol) was taken up in 1:9 methanol/acetonitrile (20 mL). N,N-diisopropylethylamine (1.1 mL, 6.35 mmol) was added dropwise followed by (trimethylsilyl)diazomethane (3.2 mL, 6.35 mmol). The reaction was stirred until the bubbling stopped (20 min) and the reaction was quenched with water. The water was extracted 3× with methylene chloride, dried over Na2SO4, filtered, and concentrated in vacuo to give 5-tert-butyl-2-methoxy-3-nitro-benzonitrile (0.531 g, 99%) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07592332B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-849f861350ba48708559e41fb9aaf381 |
| Source note | uspto-grants-2009_09 |