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Sulfuric Acid → 1,1,4,4,5,7-Hexamethyl-1,2,3,4-tetrahydronaphthalene

HRID 486415
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HRID 486415 반응식
[CH2:1](Cl)[C:2](=[CH2:4])[CH3:3].OS(O)(=O)=O.[C:11]1([CH3:18])[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[CH:12]=1>>[CH3:3][C:2]1([CH3:4])[C:15]2[C:16](=[C:11]([CH3:18])[CH:12]=[C:13]([CH3:17])[CH:14]=2)[C:2]([CH3:4])([CH3:3])[CH2:1][CH2:1]1
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참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 7929M-XyleneHCID 112413-Chloro-2-methyl-1-propene

생성물 1

HCID 138132891,1,4,4,5,7-Hexamethyl-1,2,3,4-tetrahydronaphthalene

반응 조건

온도
20 °C

실험 절차

The starting material 1,1,4,4,5,7-hexamethyl-1,2,3,4-tetrahydronaphthalene is prepared by substantially following the procedures of Fehr et al., U.S. Pat. No. 5,162,588. Specifically, in a 1 liter three-neck flask, equipped with a mechanical stirrer and kept under nitrogen, 150.0 g of methallyl chloride are slowly (2 hrs) added to a mixture of meta-xylene (490.9 g) and H2SO4 (30.0 g), while the temperature is maintained at 20° C. After 3 hrs, the H2SO4 is decanted and the organic phase is washed with, in succession, water, an aqueous solution saturated with NaHCO3, and an aqueous solution saturated with NaCl. The excess of meta-xylene is recovered through distillation, and the residue is distilled. A mixture of two isomers, 1-(2-chloro-1,1-dimethylethyl)-2,4-dimethylbenzene and 1-(2-chloro-1,1-dimethylethyl)-3,5-dimethylbenzene, is obtained.

후처리

  1. customSpecifically, in a 1 liter three-neck flask, equipped with a mechanical stirrer
  2. custom(2 hrs)
  3. customthe H2SO4 is decanted
  4. washthe organic phase is washed with, in succession, water
  5. distillationThe excess of meta-xylene is recovered through distillation
  6. distillationthe residue is distilled
  7. additionA mixture of two isomers, 1-(2-chloro-1,1-dimethylethyl)-2,4-dimethylbenzene and 1-(2-chloro-1,1-dimethylethyl)-3,5-dimethylbenzene
  8. customis obtained

출처 및 근거

ORD 기록
ord-45509428ef93463e961b3c9837060dea
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05292719

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