Toluene → HCID 54505258, 화합물

HRID 361970

반응식

HRID 361970 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4](Cl)=[O:5].[CH3:12][C:13]1[CH:14]=[C:15]([O:19][CH3:20])[CH:16]=[CH:17][CH:18]=1.C1(C)C=CC=CC=1>[Fe](Cl)(Cl)Cl.O>[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4]([C:18]1[CH:17]=[CH:16][C:15]([O:19][CH3:20])=[CH:14][C:13]=1[CH3:12])=[O:5]

참가 물질

6

반응물 3

HCID 1140TolueneHCID 75303-MethoxytolueneHCID 783922,6-Dichlorobenzoyl chloride

생성물 1

HCID 54505258HCID 54505258, 화합물

시약·촉매·용매 2

HCID 24380Iron chloride (FeCl3)촉매HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

A mixture of 2,6-dichlorobenzoylchloride (5.24 g; 25 mmol), 3-methylanisole(2.44 g; 20 mmol) and iron(III)chloride (20 mg) is heated to 100° C.for 45 minutes with stirring. After cooling, toluene is added, the mixture is shaken with water, the organic phase is dried and the solvent is evaporated. The reaction product is purified chromatograpically (flash column with 70 g of silicagel; elution with petrolether/toluene changing from 75:25 to 40:60 (v/v)). After evaporation the residue from the main fraction is treated with petrolether to give white crystals (1.33 g; 22.5%y); mp. 89° C.

후처리

  1. temperatureAfter cooling
  2. customthe organic phase is dried
  3. customthe solvent is evaporated
  4. customThe reaction product is purified chromatograpically
  5. wash(flash column with 70 g of silicagel; elution with petrolether/toluene changing from 75:25 to 40:60 (v/v))
  6. customAfter evaporation the residue from the main fraction
  7. additionis treated with petrolether
  8. customto give white crystals (1.33 g; 22.5%y)

출처 및 근거

ORD 기록
ord-03ef2cdb6e0045279aa073cd8d8b37ea
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866722

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