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Hydrochloric Acid → 2-Cyclopropyl-6-methylphenol

HRID 1866837
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HRID 1866837 반응식
[Mg].C([O:5][C:6]1[C:11]([CH3:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH:13](Br)[CH2:14][CH2:15]Br)(=O)C.Cl>C1COCC1>[CH:13]1([C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([CH3:12])[C:6]=2[OH:5])[CH2:14][CH2:15]1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 5462224MagnesiumHCID 119598052-(1,3-Dibromopropyl)-6-methylphenyl acetate

생성물 1

HCID 229399512-Cyclopropyl-6-methylphenol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

반응 조건

온도
75 °C

실험 절차

A 200 ml four-necked round-bottomed flask was equipped with a magnetic stirrer bar, a thermometer and a drying tube. Magnesium (498 mg, 20.5 mmol) and anhydrous THF (7 ml) were added thereto under a nitrogen atmosphere. The mixture was heated in an oil bath of 75° C. for 15 minutes (temperature of the mixture was 62-64° C.). Subsequently, the mixture was heated in an oil bath of 75° C. and a solution of 2-(1,3-dibromopropyl)-6-methylphenyl acetate (6.00 g, 17.1 mmol or less) in THF (21 ml) was added thereto over 20 minutes. The temperature of the mixture was raised to 70° C. After the mixture was stirred in an oil bath of 75° C. for 3 hours, the mixture was cooled and 6M hydrochloric acid (7.13 ml, 42.8 mmol) was added thereto over 5 minutes. After the mixture was stirred at room temperature for 1 hour, it was transferred to a 200 ml round bottom flask and most of THF was distilled off under reduced pressure. Methanol (15 ml) was added to the residue and the obtained mixture was stirred under heating at reflux for 9 hours. The mixture was cooled and methanol was distilled off under reduced pressure. Water (8 ml) was added to the residue and it was extracted with toluene (25 ml and 15 ml). The organic layer was combined and washed with water (20 ml), followed by concentration to obtain 2.69 g of a crude product of 2-cyclopropyl-6-methylphenol.

후처리

  1. customA 200 ml four-necked round-bottomed flask was equipped with a magnetic stirrer bar
  2. customwas 62-64° C.
  3. temperatureSubsequently, the mixture was heated in an oil bath of 75° C.
  4. temperatureThe temperature of the mixture was raised to 70° C
  5. temperaturethe mixture was cooled
  6. waitover 5 minutes
  7. stirringAfter the mixture was stirred at room temperature for 1 hour
  8. distillationwas distilled off under reduced pressure
  9. additionMethanol (15 ml) was added to the residue
  10. stirringthe obtained mixture was stirred
  11. temperatureunder heating
  12. temperatureat reflux for 9 hours
  13. temperatureThe mixture was cooled
  14. distillationmethanol was distilled off under reduced pressure
  15. additionWater (8 ml) was added to the residue and it
  16. extractionwas extracted with toluene (25 ml and 15 ml)
  17. washwashed with water (20 ml)
  18. concentrationfollowed by concentration

출처 및 근거

ORD 기록
ord-9bd41540c71f4bec814ac2f50c2fa9ee
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07629494B2

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