Toluene → 1,4-dihydro-3H-2-benzopyran-3-one

HRID 842326

反応式

HRID 842326 の反応式
[C:1]([O:4][CH2:5][CH3:6])(=[O:3])[CH3:2].[C:7]1(C)[CH:12]=[CH:11]C=[CH:9][CH:8]=1.C1(C)C(C)=CC=CC=1.C(C1C=CC=CC=1)C>C(Cl)Cl>[CH2:5]1[C:6]2[C:9](=[CH:8][CH:7]=[CH:12][CH:11]=2)[CH2:2][C:1](=[O:3])[O:4]1

参加物

6

反応物 4

HCID 1140TolueneHCID 7237O-XyleneHCID 7500EthylbenzeneHCID 8857Ethyl Acetate

生成物 1

HCID 780921,4-dihydro-3H-2-benzopyran-3-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

After the reaction, recovery of isochromanones can be carried out by concentration of reaction mixture or extraction with an organic solvent such as ethyl acetate, toluene, xylene, ethylbenzene, or methylene chloride. When the reaction mixture is separated into two layers, i.e., a water layer and a product layer, depending on the target isochromanones, it is possible to separate and remove the water layer. In particular, when the product is 3-isochromanone, the product layer is liquid at 85° C. or higher, so that solubility in water is low and the target compound can be recovered by separation operation. Further, distillation and purification under reduced pressure can give rise to highly pure 3-isochromanone.

後処理

  1. customWhen the reaction mixture is separated into two layers, i.e.
  2. customto separate
  3. customremove the water layer
  4. customat 85° C.
  5. customthe target compound can be recovered by separation operation
  6. distillationFurther, distillation and purification under reduced pressure

出典と根拠

ORDレコード
ord-bdf2f6d3faaf446184656218d3c84c1f
出典データセット
uspto-grants-2002_04
特許番号
US06372921B1

関連ノート

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