Potassium Carbonate → 1,3-Bis[4-(4-nitro-6-fluorophenoxy)-alpha, alpha-dimethylbenzyl]benzene

HRID 1109676

반응식

HRID 1109676 반응식
[F:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1F.[OH:12][C:13]1[CH:37]=[CH:36][C:16]([C:17]([C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([C:29]3[CH:34]=[CH:33][C:32]([OH:35])=[CH:31][CH:30]=3)([CH3:28])[CH3:27])[CH:21]=2)([CH3:19])[CH3:18])=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N+:9]([C:4]1[CH:3]=[C:2]([F:1])[C:7]([O:12][C:13]2[CH:14]=[CH:15][C:16]([C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([CH3:27])([CH3:28])[C:29]4[CH:30]=[CH:31][C:32]([O:35][C:7]5[C:2]([F:1])=[CH:3][C:4]([N+:9]([O-:11])=[O:10])=[CH:5][CH:6]=5)=[CH:33][CH:34]=4)[CH:21]=3)([CH3:19])[CH3:18])=[CH:36][CH:37]=2)=[CH:6][CH:5]=1)([O-:11])=[O:10]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1230531,2-Difluoro-4-nitrobenzeneHCID 3292100Phenol, 4,4'-[1,3-phenylenebis(1-methylethylidene)]bis-

생성물 1

HCID 867479171,3-Bis[4-(4-nitro-6-fluorophenoxy)-alpha, alpha-dimethylbenzyl]benzene수율 104.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

To a reaction vessel equipped with a thermometer, reflux condenser and a stirrer, 200 g of N,N-dimethylformamide (DMF), 65 g (0.409 mol) of 3,4-difluoronitrobenzene, 69.1 g (0.199 mol) of 1,3-bis(4-hydroxycumyl) benzene and 33.1 g (0.239 mol) of potassium carbonate were charged and warmed to 80° C. with stirring. After aging the mixture at 80° C. for 6 hours, inorganic salts was removed by filtration. The filtrate was mixed with 50 ml of water and cooled to the room temperature. The precipitated crystal was filtered and slugged with isopropyl alcohol to obtain 129.4 g (97% yield) of 1,3-bis[4-(4-nitro-6-fluorophenoxy)-α, α-dimethylbenzyl]benzene having a melting point of 150.7°~151.8° C.

후처리

  1. customTo a reaction vessel equipped with a thermometer
  2. temperaturereflux condenser and a stirrer
  3. customat 80° C.
  4. customfor 6 hours
  5. custominorganic salts was removed by filtration
  6. additionThe filtrate was mixed with 50 ml of water
  7. temperaturecooled to the room temperature
  8. filtrationThe precipitated crystal was filtered

출처 및 근거

ORD 기록
ord-7dd67369127c40c986d251e420e58aa8
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05321096

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