Potassium Carbonate → 4-[o-(1-Propenyl)phenoxy]benzophenone

HRID 414149

반응식

HRID 414149 반응식
[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:25]=[CH:24][C:15]([C:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[O:17])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+].CN1CCCC1=O>C1(C)C=CC=CC=1>[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[O:10][C:21]1[CH:22]=[CH:23][C:18]([C:16]([C:15]2[CH:24]=[CH:25][CH:12]=[CH:13][CH:14]=2)=[O:17])=[CH:19][CH:20]=1)=[CH:2][CH3:3]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 156242-AllylphenolHCID 676634-Fluorobenzophenone

생성물 1

HCID 544155974-[o-(1-Propenyl)phenoxy]benzophenone

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

o-Allylphenol (33.5 g), 4-fluorobenzophenone (50.05 g), potassium carbonate (24.20 g), dry N-methylpyrrolidone (160 ml) and toluene (60 ml) are placed in a 3-necked 500 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 (50 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 4-[o-(1-propenyl)phenoxy]benzophenone as a light yellow melt. The yield is 73 g.

후처리

  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 (50 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

출처 및 근거

ORD 기록
ord-33fb45e1eee9447baa9e133e19e2a1bc
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04789704

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