Water → 3-Chloro-6-(methylsulfonyl)-2,4-dinitrotoluene

HRID 903482노트

반응식

HRID 903482 반응식
[CH3:1][S:2]([C:5]1[C:6]([CH3:18])=[C:7]([N+:15]([O-:17])=[O:16])[C:8](O)=[C:9]([N+:11]([O-:13])=[O:12])[CH:10]=1)(=[O:4])=[O:3].O.P(Cl)(Cl)([Cl:22])=O>CN(C)C1C=CC=CC=1>[Cl:22][C:8]1[C:7]([N+:15]([O-:17])=[O:16])=[C:6]([CH3:18])[C:5]([S:2]([CH3:1])(=[O:4])=[O:3])=[CH:10][C:9]=1[N+:11]([O-:13])=[O:12]

참가 물질

5

반응물 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 233359754-(Methylsulfonyl)-2,6-dinitro-m-cresol

생성물 1

HCID 233359733-Chloro-6-(methylsulfonyl)-2,4-dinitrotoluene

시약·촉매·용매 1

HCID 949N,N-Dimethylaniline용매

실험 절차

To a slurry of 4-(methylsulfonyl)-2,6-dinitro-m-cresol (4.9 g.) in phosphorus oxychloride (21 ml.), N,N-dimethylaniline is added at such a rate that the temperature does not exceed 34° C. When the addition is complete and the initial exotherm has subsided, the mixture is heated to 60°-65° C. and held there for 10 minutes. The reaction mixture is carefully decomposed by pouring into a ice and water mixture. The desired product as a precipitated solid (4.49 g.) is collected and recrystallized from benzene-pet ether to give a solid with m.p. of 174°-175° C. Analysis: Calcd. for C8H7ClN2O6S: C, 32.59; H, 2.37; N, 9.50; S, 10.86; Cl, 12.05. Found: C, 32.62; H, 2.37; N, 9.39; S, 10.65; Cl, 12.25.

후처리

  1. customdoes not exceed 34° C
  2. additionWhen the addition
  3. temperaturethe mixture is heated to 60°-65° C.
  4. customThe desired product as a precipitated solid (4.49 g.) is collected
  5. customrecrystallized from benzene-pet ether
  6. customto give a solid with m.p. of 174°-175° C

출처 및 근거

ORD 기록
ord-80b67d4bc5564e2b9615a0cbf620efd4
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04227913

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