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

HRID 1199366

반응식

HRID 1199366 반응식
[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]

참가 물질

3

반응물 1

HCID 926004,5-Dichlorophthalic acid

생성물 1

HCID 703344,5-Dichlorophthalic anhydride수율 87.4%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a0baddf346924f6fa2ad3ad86239dc35
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04900739

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