HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → (R)-(+)-4-tert. butoxy-3-methylbutyronitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Cyanide | HCID 8929 | — |
| Reactant | bromo ether (S)-(+)-3-tert. butoxy-2-methyl-1-bromopropane | HCID 86735108 | — |
| Solvent | Water | HCID 962 | — |
| Product | (R)-(+)-4-tert. butoxy-3-methylbutyronitrile | HCID 12923321 | 64.6% |
Reaction Steps
A mixture of 23.1 g. (0.11 mole) of bromo ether (S)-(+)-3-tert. butoxy-2-methyl-1-bromopropane and 11.07 g. (0.225 mole) of sodium cyanide in 144 ml. of methanol and 36 ml. of water was stirred and refluxed for 17 hours. After cooling, the reaction mixture was diluted with water and worked up by extraction with CH2Cl2 in the manner of Example 1. The crude product was chromatographed on 500 g. of silica gel. Elution with 9:1 parts by volume and 4:1 parts by volume hexane-ether followed by evaporative distillation gave (R)-(+)-4-tert. butoxy-3-methylbutyronitrile (11.03 g.; 64.5%) as a colorless liquid, b.p. 88°-90° C. (bath temperature) (11 mm Hg.); [α]25D+7.41° (c 1.8, C6H6).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04151205 |
| Source dataset | uspto-grants-1979_04 |
| ORD ID | ord-012c4d5ae5ea445d8b3030b7309cc627 |
| Source note | uspto-grants-1979_04 |