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

HRID 842325

反応式

HRID 842325 の反応式
[C:1]([O:4][CH2:5][CH3:6])(=[O:3])[CH3:2].C(Cl)Cl.[C:10]1(C)[CH:15]=[CH:14]C=[CH:12][CH:11]=1.C(C1C=CC=CC=1)C>O.C1(C)C(C)=CC=CC=1>[CH2:5]1[C:6]2[C:12](=[CH:11][CH:10]=[CH:15][CH:14]=2)[CH2:2][C:1](=[O:3])[O:4]1

参加物

7

反応物 4

HCID 1140TolueneHCID 6344DichloromethaneHCID 7500EthylbenzeneHCID 8857Ethyl Acetate

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7237O-Xylene溶媒

実験手順

Recovery of isochromanones after the reaction is possible by concentration of reaction mixture or extraction with organic solvents such as ethyl acetate, methylene chloride, toluene, xylene, and ethylbenzene. Depending on the target isochromanones, when there are two layers, i.e., water layer and product layer, it is possible to separate the water layer and remove it. In particular, when the product is 3-isochromanone, the product layer is liquid at 85° C. or higher, and the solubility in water is low so that the target compound can be recovered by the operation of separation. Further, it is possible to obtain high purity 3-isochromanone by distillation purification under reduced pressure.

後処理

  1. customto separate the water layer
  2. customremove it
  3. customat 85° C.
  4. customcan be recovered by the operation of separation

出典と根拠

ORDレコード
ord-08c3f210f5904025865c4c3628dbaab9
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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