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Acetic Acid → 2-Methyl-cyclohex-2-en-1-yl acetate

HRID 742817
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HRID 742817 반응식
[CH3:1][C:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=1.C.OO.[C:11]([OH:14])(=[O:13])[CH3:12]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(=O)C=CC(=O)C=C1>[C:11]([O:14][CH:3]1[CH2:4][CH2:5][CH2:6][CH:7]=[C:2]1[CH3:1])(=[O:13])[CH3:12]
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참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 297MethaneHCID 784Hydrogen PeroxideHCID 115741-Methylcyclohexene2회

생성물 1

HCID 126351582-Methyl-cyclohex-2-en-1-yl acetate수율 50%

시약·촉매·용매 2

HCID 4650Quinone촉매
HCID 167845
palladium(II) acetate
촉매

실험 절차

Acetoxylation of 1-methylcyclohexene A 500 ml three-neck flask is charged with 15 g of 1-methylcyclohexene (0.15 moles), 150 g of acetic acid, 0.77 g of benzoquinone (7 mmoles), 1 g of active charcoal and 80 mg of palladium acetate (0.35 mmoles). The temperature is taken to 50°, then 8 g (0.17 moles) of 70% by weight hydrogen peroxide are introduced in 8 h, and the reaction is allowed to proceed for a further 2 h while maintaining the temperature at 50°. The acetic acid is then distilled (35°, 20×102Pa). The residue is distilled under vacuum (75°-80°, 15×102Pa) to provide 2-methyl-cyclohex-2-en-1-yl acetate (11 g, yield 50%).

후처리

  1. customis taken to 50°
  2. temperaturewhile maintaining the temperature at 50°
  3. distillationThe acetic acid is then distilled (35°, 20×102Pa)
  4. distillationThe residue is distilled under vacuum (75°-80°, 15×102Pa)

출처 및 근거

ORD 기록
ord-76276fc7061f418eada8083114d19b48
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05554786

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