4,5-Dichlorophthalic acid → 4,5-Dichlorophthalic anhydride

HRID 1199366

反応式

HRID 1199366 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5](=[CH:9][C:10]=1[Cl:11])[C:6]([OH:8])=O>C(OC(=O)C)(=O)C>[Cl:11][C:10]1[CH:9]=[C:5]2[C:6](=[O:8])[O:14][C:12](=[O:13])[C:4]2=[CH:3][C:2]=1[Cl:1]

参加物

3

反応物 1

HCID 926004,5-Dichlorophthalic acid

生成物 1

HCID 703344,5-Dichlorophthalic anhydride収率 87.4%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

A suspension of 4,5-dichlorophthalic acid [(XVII), X=4-Cl, Y=5-Cl, 50.0 g, 0.213 mol] and acetic anhydride (70 mL) was heated to reflux until dissolution occurred. A distilling head was then attached and 30 mL of distillate was removed. The solution was cooled to room temperature whereupon a precipitate appeared. This solid was filtered, washed with anhydrous ether and dried in vacuo to provide the product (40.4 g, 87%) as a tan solid, m.p. 189°-192° C.

後処理

  1. temperaturewas heated
  2. temperatureto reflux until dissolution
  3. custom30 mL of distillate was removed
  4. filtrationThis solid was filtered
  5. washwashed with anhydrous ether
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-a0baddf346924f6fa2ad3ad86239dc35
出典データセット
uspto-grants-1990_02
特許番号
US04900739

関連ノート

読み込み中…