Sodium Bicarbonate → HCID 178432730、化合物

HRID 216318

反応式

HRID 216318 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 178432730HCID 178432730、化合物

試薬・触媒・溶媒 2

HCID 10313229titanium(III) trichloride触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-322421c136d749628ace9adadd934aeb
出典データセット
uspto-grants-2012_06
特許番号
US08193228B2

関連ノート

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