Anisole → 4-Methoxycarbonyl-2'-methoxybenzophenone

HRID 1654717ノート

反応式

HRID 1654717 の反応式
[C:1]1([O:7][CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[CH3:10][O:11][C:12](=[O:22])[C:13]1[CH:21]=[CH:20][C:16]([C:17](O)=[O:18])=[CH:15][CH:14]=1.[Cl-].[Al+3].[Cl-].[Cl-]>>[CH3:10][O:11][C:12]([C:13]1[CH:21]=[CH:20][C:16]([C:17]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=2[O:7][CH3:8])=[O:18])=[CH:15][CH:14]=1)=[O:22]

参加物

4

反応物 3

HCID 7519AnisoleHCID 6451240Aluminum(III) ChlorideHCID 53442854Terephthalic acid monomethylester chloride

生成物 1

HCID 224082434-Methoxycarbonyl-2'-methoxybenzophenone

実験手順

To a mixture of anisole (216 g) and terephtalic acid-methyl ester-chloride (99 g) was added aluminium chloride (200 g) at 0° C. in an amount of 1/3 to 1/4 at a time. In that case, temperature was kept to 25° C. or less, and it took from 45 minutes to 1 hour for addition. The temperature returned to room temperature after 30 minutes from termination of addition, and after stirring for 1.5 hours to 2 hours, the pink colored precipitate was obtained by pouring ice-water. The precipitate was separated by filtration, dried with water and washed with methanol. Methanol washings were concentrated under reduced pressure, and washed with a small amount of methanol to give the title compound.

後処理

  1. customwas kept to 25° C. or less
  2. additionit took from 45 minutes to 1 hour for addition
  3. additionThe temperature returned to room temperature after 30 minutes from termination of addition
  4. customthe pink colored precipitate was obtained
  5. customThe precipitate was separated by filtration
  6. dry with materialdried with water
  7. washwashed with methanol
  8. concentrationMethanol washings were concentrated under reduced pressure
  9. washwashed with a small amount of methanol

出典と根拠

ORDレコード
ord-297a111bb96244248112a9b2900445ae
出典データセット
uspto-grants-1995_04
特許番号
US05409928

反応ノート

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