4,4'-Difluorobenzophenone → HCID 86742606、化合物

HRID 414150

反応式

HRID 414150 の反応式
[CH2:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[OH:10])[CH:2]=[CH2:3].F[C:12]1[CH:26]=[CH:25][C:15]([C:16]([C:18]2[CH:23]=[CH:22][C:21](F)=[CH:20][CH:19]=2)=[O:17])=[CH:14][CH:13]=1.F[C:28]1[CH:41]=[CH:40][C:31]([C:32]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)=[O:33])=[CH:30][CH:29]=1.C(=O)([O-])[O-:43].[K+].[K+]>C1(C)C=CC=CC=1.CN1CCCC1=O>[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[O:10][C:12]1[CH:26]=[CH:25][C:15]([C:16]([C:18]2[CH:23]=[CH:22][C:21]([O:43][C:40]3[CH:41]=[CH:28][CH:29]=[CH:30][C:31]=3[CH:32]=[CH:34][CH3:35])=[CH:20][CH:19]=2)=[O:17])=[CH:14][CH:13]=1)=[CH:2][CH3:3].[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[O:10][C:37]1[CH:38]=[CH:39][C:34]([C:32]([C:31]2[CH:40]=[CH:41][CH:28]=[CH:29][CH:30]=2)=[O:33])=[CH:35][CH:36]=1)=[CH:2][CH3:3]

参加物

7

反応物 4

HCID 95824,4'-DifluorobenzophenoneHCID 11430Potassium CarbonateHCID 156242-AllylphenolHCID 676634-Fluorobenzophenone

生成物 1

HCID 86742606HCID 86742606、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
100 °C

実験手順

o-Allylphenol (52.2 g), 4,4'-difluorobenzophenone (35 g), 4-fluorobenzophenone (13.8 g), potassium carbonate (37.75 g), dry N-methylpyrrolidone (200 ml) and toluene (75 ml) are placed in a 3-necked 1500 ml flask fitted with a stirrer, reflex condensor and thermometer and the mixture is heated under nitrogen to a temperature between 155°-160° C. and stirred for 3 hours. Water and toluene are separated via a Dean Stark trap and finally after 3 hours the reaction mixture reaches a temperature of 160° C. The mixture is cooled to 100° C. and a 1:1 mixture of toluene/water (400 ml) is added while stirring. After phase separation the aqueous layer is washed with toluene (100 ml) and the combined toluene layers are washed 4 times with water (150 ml). The toluene phase is dried over sodium sulphate and toluene distilled off by use of a rotary evaporator finally in vacuum leaving a 4,4'-bis[o-(1-propenyl)phenoxy]benzophenone/4-[o-(1-propenyl)phenoxy]benzophenone mixture as a light yellow melt. The yield is 89 g.

後処理

  1. customfitted with a stirrer
  2. temperaturereflex condensor and thermometer and the mixture is heated under nitrogen to a temperature between 155°-160° C.
  3. customWater and toluene are separated via a Dean Stark trap and finally after 3 hours the reaction mixture
  4. customa temperature of 160° C
  5. additiona 1:1 mixture of toluene/water (400 ml)
  6. additionis added
  7. stirringwhile stirring
  8. customAfter phase separation the aqueous layer
  9. washis washed with toluene (100 ml)
  10. washthe combined toluene layers are washed 4 times with water (150 ml)
  11. dry with materialThe toluene phase is dried over sodium sulphate and toluene
  12. distillationdistilled off by use of a rotary evaporator finally in vacuum

出典と根拠

ORDレコード
ord-eb6fcc868bd5423189fa7be8c72096f1
出典データセット
uspto-grants-1988_12
特許番号
US04789704

関連ノート

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