Dimethylformamide → 2,2',4,4'-Tetrahydroxybenzophenone

HRID 2395

반응식

HRID 2395 반응식
[Al+3].[Cl-].[Cl-].[Cl-].CN(C)C=O.C[O:11][C:12]1[CH:29]=[C:28]([O:30]C)[CH:27]=[CH:26][C:13]=1[C:14]([C:16]1[CH:21]=[CH:20][C:19]([O:22]C)=[CH:18][C:17]=1[O:24]C)=[O:15]>O>[OH:11][C:12]1[CH:29]=[C:28]([OH:30])[CH:27]=[CH:26][C:13]=1[C:14]([C:16]1[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][C:17]=1[OH:24])=[O:15]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 815404Bis(2,4-dimethoxyphenyl)methanoneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 85712,2',4,4'-Tetrahydroxybenzophenone

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
30 °C

실험 절차

440 g (3.30 mol) of AlCl3 were stirred into 120 g (1.64 mol) of dimethylformamide in such a way that the temperature remained below 160° C. After cooling to 30° C., 60.5 g (0.20 mol) of 2,2',4,4'-tetramethoxybenzophenone were introduced into the mixture, which was easily stirrable. The mixture was stirred at about 50°-52° C. for 4.5 hours and then added to 1.8 l of water to which 3 g of active carbon had been added. The hydrolyzate was filtered at about 95° C., and then 65 g of concentrated hydrochloric acid were added to the filtrate. The precipitate was filtered off with suction at 25° C., washed with water and dried at 125° C. under reduced pressure.

후처리

  1. customremained below 160° C
  2. additionhad been added
  3. filtrationThe hydrolyzate was filtered at about 95° C.
  4. addition65 g of concentrated hydrochloric acid were added to the filtrate
  5. filtrationThe precipitate was filtered off with suction at 25° C.
  6. washwashed with water
  7. customdried at 125° C. under reduced pressure

출처 및 근거

ORD 기록
ord-8a215651ccfd41dd9aa2a1416e37b1fc
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728888

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