Sodium Bicarbonate → HCID 178432730, 화합물

HRID 216318

반응식

HRID 216318 반응식
[CH3:1][C:2]([CH3:12])([CH3:11])[CH2:3][C:4]1[N:5]=[C:6]([CH3:10])[N:7](O)[CH:8]=1.C(=O)(O)[O-].[Na+]>CO.[Cl-].[Ti+3].[Cl-].[Cl-]>[CH3:1][C:2]([CH3:12])([CH3:11])[CH2:3][C:4]1[N:5]=[C:6]([CH3:10])[NH:7][CH:8]=1

참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 686676414-(2,2-dimethylpropyl)-2-methyl-1H-imidazol-1-ol

생성물 1

HCID 178432730HCID 178432730, 화합물

시약·촉매·용매 2

HCID 10313229titanium(III) trichloride촉매HCID 887Methanol용매

실험 절차

Titanium (III) chloride (30% weight solution in 2N HCl) (600 mL, 1.5 mol) was added to an ambient temperature solution of 4-(2,2-dimethylpropyl)-2-methyl-1H-imidazol-1-ol (ca. 0.56 mmol) in methanol (1200 mL). After stirring at ambient temperature for a few days, the reaction mixture was basified with saturated aqueous sodium bicarbonate until the black solution turned white. The reaction mixture was extracted with ether. The combined organic extracts were washed with brine, dried (magnesium sulfate), filtered and concentrated in vacuo. Chromatography over silica eluting with 10-20% ethyl acetate/hexane afforded 4-(2,2-dimethylpropyl)-2-methyl-1H-imidazole.

후처리

  1. extractionThe reaction mixture was extracted with ether
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried (magnesium sulfate)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-322421c136d749628ace9adadd934aeb
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193228B2

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