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4-Chlorophenol → 2-[(4-Chlorophenoxy)methyl]thiophene

HRID 568362
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HRID 568362 반응식
Br[CH2:2][C:3]1[S:4][CH:5]=[CH:6][CH:7]=1.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:2][C:3]2[S:4][CH:5]=[CH:6][CH:7]=2)=[CH:11][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 46844-ChlorophenolHCID 11430Potassium CarbonateHCID 118299782-(Bromomethyl)thiophene

생성물 1

HCID 137869942-[(4-Chlorophenoxy)methyl]thiophene

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 51.75 g (0.29 m) of 2-bromomethylthiophene and 38.6 g (0.3 m) of 4-chlorophenol in 400 ml of acetonitrile was added, all at once, 38.6 g of powdered potassium carbonate. The resulting mixture was stirred and heated at reflux for one (1) hour. The solvent was removed by evaporation under reduced pressure and 400 ml of water was added to the residue. The resulting aqueous mixture was extracted three times with 200 ml portions of ether. The organic extracts were combined and then washed sequentially with 50 ml of a 10 percent sodium hydroxide solution, 300 ml of water and 300 ml of a saturated sodium chloride solution. The extracts were dried over magnesium sulfate and the solvent removed by evaporation under reduced pressure. The residue was an orange oil which slowly solidified upon standing. Distillation of the residue gave a main fraction boiling at 96°-100° C. at 0.01 millimeter of mercury. The crude product slowly crystallized and was purified by recrystallization from hexane. The (4-chlorophenoxy)methylthiopene product, a white solid, was recovered in a yield of 41 g (63 percent of theoretical) and melted at 45°-47° C.

후처리

  1. temperatureheated
  2. customThe solvent was removed by evaporation under reduced pressure and 400 ml of water
  3. additionwas added to the residue
  4. extractionThe resulting aqueous mixture was extracted three times with 200 ml portions of ether
  5. washwashed sequentially with 50 ml of a 10 percent sodium hydroxide solution, 300 ml of water and 300 ml of a saturated sodium chloride solution
  6. dry with materialThe extracts were dried over magnesium sulfate
  7. customthe solvent removed by evaporation under reduced pressure
  8. distillationDistillation of the residue
  9. customgave a main fraction boiling at 96°-100° C. at 0.01 millimeter of mercury
  10. customThe crude product slowly crystallized
  11. customwas purified by recrystallization from hexane
  12. customThe (4-chlorophenoxy)methylthiopene product, a white solid, was recovered in a yield of 41 g (63 percent of theoretical) and melted at 45°-47° C.

출처 및 근거

ORD 기록
ord-92174a4aefd143258fbfdbeb0ae51237
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04728657

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