Toluene → HCID 54505258、化合物

HRID 361970

反応式

HRID 361970 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 54505258HCID 54505258、化合物

試薬・触媒・溶媒 2

HCID 24380Iron chloride (FeCl3)触媒HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-03ef2cdb6e0045279aa073cd8d8b37ea
出典データセット
uspto-grants-1999_02
特許番号
US05866722

関連ノート

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