4-Chloro-3,5-dinitrobenzoic acid → 4-Chloro-3,5-dinitrobenzoyl chloride

HRID 236945

반응식

HRID 236945 반응식
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6](O)=[O:7])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].P(Cl)(Cl)(Cl)(Cl)[Cl:18]>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([Cl:18])=[O:7])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15]

참가 물질

3

반응물 2

HCID 83774-Chloro-3,5-dinitrobenzoic acidHCID 24819Phosphorus pentachloride

생성물 1

HCID 234515644-Chloro-3,5-dinitrobenzoyl chloride수율 72%

실험 절차

A mixture of 75.75 gm. (0.307 mole) of 4-chloro-3,5-dinitrobenzoic acid and 64.0 gm. (0.307 mole) of phosphorus pentachloride is heated at reflux for ninety minutes and cooled to room temperature. The phosphorus oxychloride is removed by distillation in vacuo. The residue is washed with Skellysolve "B" and the solvent removed by decantation. The oily residue is recrystallized from benzene-cyclohexane. There is obtained 58.2 gm (72%) of tan needles melting at 55°-57°.

후처리

  1. additionA mixture of 75.75 gm
  2. temperatureat reflux for ninety minutes
  3. customThe phosphorus oxychloride is removed by distillation in vacuo
  4. washThe residue is washed with Skellysolve "B"
  5. customthe solvent removed by decantation
  6. customThe oily residue is recrystallized from benzene-cyclohexane

출처 및 근거

ORD 기록
ord-6065e3b4817a411fa4daeb65713c57b8
출처 데이터셋
uspto-grants-1979_06
특허 번호
US04159278

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