HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 13706729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 54460680 | HCID 54460680 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 13706729 | HCID 13706729 | 76% |
Reaction Steps
To a solution of 71 g of 2-fluoro-2-methyl hexanoic acid ethyl ester in 500 ml of glyme was added 1.1 eq. of 1 N sodium hydroxide solution. After stirring for 3.5 hr., the glyme was removed under vacuum, the residue extracted with ether and the aqueous layer acidified. The mixture was then extracted with pentane and the pentane solution dried. The solvent was then removed under vacuum to give 61 g of crude acid. The crude acid was treated with 156 g of oxalyl chloride and the solution stirred at room temperature for 1.5 hr and then heated at 65° for 1.5 hr. The excess oxalyl chloride was then removed under vacuum and the residue distilled to give 51 g of 2-fluoro-2-methylhexanoyl chloride b.p. 60° (25-30 mmHg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04211724 |
| Source dataset | uspto-grants-1980_07 |
| ORD ID | ord-432657f3459f482c989861237c1dd5a3 |
| Source note | uspto-grants-1980_07 |