2-Methyl-2-butene → HCID 178454351、化合物

HRID 1875077ノート

反応式

HRID 1875077 の反応式
Cl([O-])=O.[Na+].[OH2:5].P([O-])(O)(O)=O.[Na+].[CH3:12][C:13]([O:16][C:17]([N:19]([C:27]1[NH:28][CH:29]=[C:30]([CH:32]=[O:33])[N:31]=1)[C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])=[O:18])([CH3:15])[CH3:14].CC(=CC)C>O.C1COCC1.CC(O)(C)C>[CH3:15][C:13]([O:16][C:17]([N:19]([C:20]([O:22][C:23]([CH3:24])([CH3:25])[CH3:26])=[O:21])[C:27]1[NH:28][CH:29]=[C:30]([C:32]([OH:5])=[O:33])[N:31]=1)=[O:18])([CH3:12])[CH3:14]

参加物

8

反応物 4

HCID 105532-Methyl-2-buteneHCID 516949Sodium Phosphate, Monobasic, MonohydrateHCID 23668197Sodium ChloriteHCID 178454349HCID 178454349、化合物

生成物 1

HCID 178454351HCID 178454351、化合物収率 53.6%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6386tert-Butanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of sodium chlorite (0.505 g, 5.59 mmol) and sodium dihydrogenphosphate monohydrate (0.463 g, 3.35 mmol) in water (4 mL) was added to a solution of bis(1,1-dimethylethyl)(4-formyl-1H-imidazol-2-yl)imidodicarbonate (0.174 g, 0.559 mmol), 2-methyl-2-butene (2M in THF) (3.49 mL, 6.99 mmol), t-BuOH (2 mL) and THF (6 mL). The mixture was stirred at RT overnight. The reaction mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was evaporated. The residue was triturated with ether and the resulting white solid was dried under vacuum to give 0.098 g (53%) of the title compound. MS m/z 326 (M−1).

後処理

  1. extractionThe reaction mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customthe solvent was evaporated
  4. customThe residue was triturated with ether
  5. customthe resulting white solid was dried under vacuum

出典と根拠

ORDレコード
ord-aad38660bad042f0a60e49009d4d24f6
出典データセット
uspto-grants-2012_11
特許番号
US08304419B2

反応ノート

読み込み中…