Methanol → 1,3-Di-tert-butylbenzene

HRID 2061956노트

반응식

HRID 2061956 반응식
CS(O[C:6]1[CH:11]=[CH:10][C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:8][C:7]=1[C:16]([CH3:19])([CH3:18])[CH3:17])(=O)=O.C([O-])=O.[Li+].CO>[Pd].[C].O>[C:12]([C:9]1[CH:10]=[CH:11][CH:6]=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:8]=1)([CH3:15])([CH3:14])[CH3:13]

참가 물질

6

반응물 3

HCID 887MethanolHCID 23680280Lithium formateHCID 445427162,4-Di-tert-butylphenyl methanesulfonate

생성물 1

HCID 1368101,3-Di-tert-butylbenzene수율 75.1%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매2회HCID 962Water용매

실험 절차

Using the thus-obtained, regenerated Pd/carbon (10 g), the same reaction as in Example II-1 was carried out in a nitrogen atmosphere under normal pressure at 25° C., in which, however, 2,4-di-tert-butylphenyl methanesulfonate (100 g, 0.35 mols), lithium formate (37 g, 0.70 mols) and methanol (600 g) were used. Water (20 mL) was added to the reaction liquid and Pd/carbon was collected through filtration, and heptane (100 g) was added to the filtrate. The organic layer obtained after extraction was concentrated under reduced pressure to give crude 1,3-di-tert-butylbenzene (50 g, yield 75% by mass).

후처리

  1. customthe same reaction as in Example II-1
  2. customwas carried out in a nitrogen atmosphere under normal pressure at 25° C., in which
  3. filtrationwas collected through filtration, and heptane (100 g)
  4. additionwas added to the filtrate
  5. customThe organic layer obtained
  6. extractionafter extraction
  7. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6c0860746d36495db6d05fdabf44a465
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08283508B2

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