Anisole → 4-Methoxycarbonyl-2'-methoxybenzophenone

HRID 1654717노트

반응식

HRID 1654717 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

HCID 224082434-Methoxycarbonyl-2'-methoxybenzophenone

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-297a111bb96244248112a9b2900445ae
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05409928

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