2,2-Difluorosuccinic acid → 3,3-Difluorooxolane-2,5-dione

HRID 868404ノート

反応式

HRID 868404 の反応式
[F:1][C:2]([F:10])([CH2:6][C:7]([OH:9])=[O:8])[C:3](O)=[O:4]>FC(F)(F)C(OC(=O)C(F)(F)F)=O>[F:1][C:2]1([F:10])[CH2:6][C:7](=[O:9])[O:8][C:3]1=[O:4]

参加物

3

反応物 1

HCID 695812,2-Difluorosuccinic acid

生成物 1

HCID 131892433,3-Difluorooxolane-2,5-dione

試薬・触媒・溶媒 1

HCID 9845Trifluoroacetic anhydride溶媒

実験手順

2,2-Difluorosuccinic acid (120 g, 0.78 moles) and trifluoroacetic anhydride (540 mL) are refluxed (bath temperature 80° C.) for 2 hours. Most of the rifluoroacetic acid is distilled utilizing a short Vigreux column, the final traces are removed under vacuum (12 mm Hg, 50° C.) and finally by stripping twice with carbontetrachloride. The oily residue solidifies on scratching with petroleum ether. Filtration and washing with petroleum ether yields 2,2-difluorosuccinic anhydride as slightly violet crystals: 98 g (92%).

後処理

  1. distillationMost of the rifluoroacetic acid is distilled
  2. customthe final traces are removed under vacuum (12 mm Hg, 50° C.)
  3. filtrationFiltration
  4. washwashing with petroleum ether

出典と根拠

ORDレコード
ord-7e15944bc02749129a5da23f189059aa
出典データセット
uspto-grants-1988_10
特許番号
US04778926

反応ノート

読み込み中…